WO2015146935A1 - 封止シート、封止構造体及び装置 - Google Patents
封止シート、封止構造体及び装置 Download PDFInfo
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- WO2015146935A1 WO2015146935A1 PCT/JP2015/058793 JP2015058793W WO2015146935A1 WO 2015146935 A1 WO2015146935 A1 WO 2015146935A1 JP 2015058793 W JP2015058793 W JP 2015058793W WO 2015146935 A1 WO2015146935 A1 WO 2015146935A1
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- WIPO (PCT)
- Prior art keywords
- resin
- sealing sheet
- sealing
- resin part
- styrene
- Prior art date
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- H01L31/04—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof adapted as photovoltaic [PV] conversion devices
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Definitions
- the present invention relates to a sealing sheet, a sealing structure sealed with the sealing sheet, and an apparatus having the sealing sheet.
- ⁇ Organic EL elements are very sensitive to moisture, and deterioration proceeds only by absorbing moisture in the atmosphere.
- a method for completely blocking the moisture that enters from the atmosphere has been studied. For example, a method of sealing an organic EL element in order to completely block moisture, and a method of capturing moisture entering with a desiccant sheet of calcium oxide are known.
- a method of sealing an organic EL element for example, a method of sealing an organic EL element with an adhesive sealing composition film containing an isobutylene resin is known (for example, see Patent Document 1).
- the present invention has been made in view of the above circumstances.
- the sealing sheet itself is excellent in moisture penetration suppression effect.
- the present invention From the adhesive surface between the substrate (adhered body) and the sealing sheet, the present invention has been made.
- An object of the present invention is to provide a sealing sheet that is excellent in preventing moisture from entering the sealing structure, and a sealing structure that is sealed with the sealing sheet and has excellent durability under heating and humidification.
- the inventor of the present invention has a resin part (A) excellent in interfacial adhesion with a substrate (adhered body) and a resin part (B) having a low water vapor permeability and an excellent effect of suppressing water intrusion on one surface.
- the present inventors have found that a sealing sheet having a resin layer present in can solve the above-mentioned problems, and have completed the present invention.
- the resin composition forming the resin part (B) is made of at least one resin selected from butyl rubber, polyisobutylene resin, styrene copolymer, polyisoprene resin, polybutadiene resin, and polybutene resin.
- the resin composition for forming the resin part (B) comprises a polyisobutylene resin (b-1) having a mass average molecular weight of 270,000 to 600,000 and a polyisobutylene resin having a mass average molecular weight of 50,000 to 250,000 (The sealing sheet according to the above [7], comprising b-2).
- the resin composition forming the resin part (B) includes a polyisobutylene resin (b-3) having a mass average molecular weight of 20,000 or more, a styrene-butadiene-styrene triblock copolymer (SBS), styrene One selected from-(ethylene-co-butylene) -styrene triblock copolymer (SEBS), styrene-isobutylene diblock copolymer (SIB), and styrene-isobutylene-styrene triblock copolymer (SIBS)
- SEBS styrene-(ethylene-co-butylene) -styrene triblock copolymer
- SIB styrene-isobutylene diblock copolymer
- SIBS styrene-isobutylene-styrene triblock copolymer
- the encapsulating sheet of the present invention is excellent in the moisture penetration suppressing effect of the encapsulating sheet itself, and into the encapsulating structure from between the substrate (adhered body) and the encapsulating sheet when the encapsulating structure is produced. Excellent in preventing moisture from entering. Furthermore, the sealing structure formed by sealing with the sealing sheet is excellent in durability under heating and humidification.
- the encapsulating sheet of the present invention includes a resin part (A) formed from a resin composition containing one or more resins selected from acrylic resins and urethane resins, and water vapor measured according to JIS K 7129.
- the sealing sheet of the present invention having such a configuration, in addition to the effect of suppressing moisture intrusion of the entire sealing sheet by the resin portion (B) having a low water vapor transmission rate, further, with the substrate (adherent)
- the resin part (A) having good interfacial adhesion can effectively suppress moisture that can enter from between the sealing sheet and the substrate (adhered body), and the sealing structure having the sealing sheet The durability of the body and device under heating and humidification can be improved.
- At least one surface of the resin layer has, for example, a shape as shown in FIGS.
- the resin part (A) 1 and the resin part (B) 2 exist on at least one surface of the resin layer of the sealing sheet. In the configuration shown in FIG.
- the resin portion (A) 1 and the resin portion (B) 2 are arranged in a lattice pattern on the surface 101 of the resin layer of the sealing sheet, and the resin portion (A) 1 Forms a closed region 3, and a resin portion (B) 2 is formed in the closed region 3.
- the resin layer (B) 2 is arranged on the outer edge of the resin part (A) 1 on the surface 102 of the resin layer of the sealing sheet, and the resin part (B) 2 is A closed region 3 is formed, and the resin portion (A) 1 is disposed in the closed region 3.
- FIG. 1B the configuration shown in FIG.
- the resin layer (A) 1 is disposed on the outer edge portion of the resin portion (B) 2 on the surface 103 of the resin layer of the sealing sheet.
- a closed region 3 is formed, and the resin portion (B) 2 is disposed in the closed region 3.
- the surface 104 of the resin layer of the sealing sheet has a resin part (B) 2 arranged in a circle in the resin part (A) 1, and the resin part (B) 2 Forms a closed region 3, and the resin portion (A) 1 is disposed in the closed region 3.
- FIG. 1D the configuration shown in FIG.
- the resin layer (A) 1 is intermittently disposed on the outer edge of the sealing sheet so that the surface 105 of the resin layer of the sealing sheet can ensure sufficient interfacial adhesion.
- the resin part (B) 2 is arranged at a part other than each resin part (A) 1. In the configuration shown in FIG. 1 (f), the surface 106 of the resin layer of the sealing sheet has at least one side of each resin portion (A) 1 at the outer edge of the sealing sheet so as to ensure sufficient interfacial adhesion.
- the resin parts (B) 2 are arranged at portions other than the resin parts (A) 1.
- FIG.1 (e) and (f) may be sufficient, from a viewpoint which can improve the interface adhesiveness of a board
- a region 3 in which the resin portion (A) 1 or the resin portion (B) 2 is closed is formed on at least one surface of the resin layer. It is preferable that the other resin portion is present.
- positioned reversely may be sufficient.
- the ratio [(A) area / (B) area] of the total surface area of the resin part (A) 1 and the total surface area of the resin part (B) 2 on at least one surface of the resin layer is 10 / It is preferably 90 to 90/10.
- the ratio [(A) area / (B) area] is more preferably 20/80 to 80/20, still more preferably 25/75 to 75/25.
- the thickness of the resin layer is appropriately selected according to the application and the like, but is preferably 0.5 to 100 ⁇ m, more preferably 1 to 60 ⁇ m, and further preferably 3 to 40 ⁇ m.
- the thickness of the resin layer is 0.5 ⁇ m or more, good interfacial adhesion can be obtained with respect to the adherend.
- the thickness of the resin layer is 100 ⁇ m or less, it is advantageous in terms of productivity and can be an easy-to-handle sealing sheet.
- Examples of the configuration of the sealing sheet of the present invention include the embodiments shown in the cross-sectional views of FIGS. 2 (a) to 2 (d), but the sealing sheet of the present invention is not limited as long as the effects of the present invention are exhibited. It is not limited to these examples.
- As a structure of the sealing sheet of this invention as shown to Fig.2 (a) and (b), the sealing sheets 201 and 202 of the structure which has the resin layer 4 on the support body 5 are mentioned, for example.
- FIG.2 (c) the sealing sheet 203 of the structure which laminated
- the resin layer 4 is preferably provided on the support 5 as shown in FIGS. 2 (a) to 2 (c). Further, as shown in FIG. 2B, only the resin portion (B) 2 exists on the surface of the resin layer 4 on the support 5 side, and the resin portion (A) 1 exists on the other surface. And the resin layer 4 in which the resin part (B) 2 exists may be sufficient.
- the thickness of the sealing sheet of the present invention is appropriately adjusted depending on the application and the like, but is preferably 0.5 to 1000 ⁇ m, more preferably 1 to 600 ⁇ m, still more preferably 3 to 400 ⁇ m, still more preferably 5 to 200 ⁇ m.
- the components contained in the sealing sheet of the present invention will be sequentially described.
- the resin composition forming the resin part (A) used in the present invention contains one or more selected from acrylic resins and urethane resins.
- acrylic resin examples include an acrylic resin containing a structural unit derived from alkyl (meth) acrylate, but an alkyl (meth) acrylate having 4 or more carbon atoms (hereinafter also referred to as “monomer (p1)”).
- An acrylic resin containing the derived structural unit (p1) is preferred.
- the number of carbon atoms of the alkyl group contained in the monomer (p1) is preferably 4 to 20, more preferably 4 to 12, and still more preferably 4 to 6, from the viewpoint of improving the interfacial adhesion of the sealing sheet.
- the alkyl group of the monomer (p1) may be either a straight chain or a branched chain.
- Examples of the monomer (p1) include n-butyl (meth) acrylate, butyl (meth) acrylate such as isobutyl (meth) acrylate, pentyl (meth) acrylate, hexyl (meth) acrylate, 2-ethylhexyl (meth) acrylate, Examples include isooctyl (meth) acrylate, lauryl (meth) acrylate, stearyl (meth) acrylate and the like. In addition, you may use these monomers (p1) individually or in combination of 2 or more types. Among these, from the viewpoint of improving the interfacial adhesion of the sealing sheet, butyl (meth) acrylate is preferable, and n-butyl (meth) acrylate is more preferable.
- the acrylic resin is a structural unit derived from the functional group-containing monomer (p2) (hereinafter also referred to as “monomer (p2)”) together with the structural unit (p1) from the viewpoint of further improving the interfacial adhesion of the sealing sheet.
- a resin containing (p2) is preferable.
- the “functional group” of the “functional group-containing monomer (p2)” means a functional group that reacts with a cross-linking agent described later to become a cross-linking origin or a functional group having a cross-linking promoting effect.
- Examples of the monomer (p2) include a hydroxyl group-containing monomer, a carboxy group-containing monomer, an amino group-containing monomer, and an epoxy group-containing monomer. These monomers (p2) may be used alone or in combination of two or more. Among these, a hydroxyl group-containing monomer and a carboxy group-containing monomer are preferable.
- hydroxyl group-containing monomer examples include 2-hydroxyethyl (meth) acrylate, 2-hydroxypropyl (meth) acrylate, 3-hydroxypropyl (meth) acrylate, 2-hydroxybutyl (meth) acrylate, and 3-hydroxybutyl (meth) )
- hydroxyalkyl (meth) acrylates such as 4-hydroxybutyl (meth) acrylate; and unsaturated alcohols such as vinyl alcohol and allyl alcohol.
- carboxy group-containing monomer examples include ethylenically unsaturated monocarboxylic acids such as (meth) acrylic acid and crotonic acid; ethylenically unsaturated dicarboxylic acids such as fumaric acid, itaconic acid, maleic acid and citraconic acid, and anhydrides thereof. , 2-carboxyethyl methacrylate and the like.
- the content of the structural unit (p1) in all the structural units of the acrylic resin is preferably 40 to 99.9% by mass, It is preferably 60 to 99% by mass, more preferably 70 to 98% by mass, and the content of the structural unit (p2) is preferably 0.1 to 30% by mass, more preferably 0.15 to 20% by mass, More preferably, it is 0.2 to 15% by mass, and still more preferably 0.25 to 10% by mass.
- the acrylic resin may contain constituent units derived from other monomers other than the constituent units (p1) and (p2) as long as the content ratios of the constituent units (p1) and (p2) are satisfied.
- Other monomers can be selected from monomers copolymerizable with acrylic monomers, and examples thereof include alkyls having 1 to 3 carbon atoms such as methyl (meth) acrylate, ethyl (meth) acrylate, and propyl (meth) acrylate.
- vinyl monomers other than those listed as monomers (p2) such as alkyl (meth) acrylate monomers having a group, styrene, ⁇ -methylstyrene, vinyl toluene, vinyl formate, vinyl acetate, acrylonitrile, acrylamide and the like.
- the mass average molecular weight (Mw) of the acrylic resin is preferably 250,000 to 1,500,000, more preferably 350,000 to 1,300,000, still more preferably 450,000 to 1,100,000, and even more preferably 650,000 to 1,50,000.
- the urethane resin used in the present invention is not particularly limited as long as it is a polymer having at least one of a urethane bond and a urea bond in the main chain and / or side chain.
- polyol (x1) and polyvalent isocyanate Urethane obtained by reacting the compound (x2) with the urethane prepolymer ( ⁇ 1) or the urethane prepolymer ( ⁇ 1) and further subjecting it to a chain extension reaction using a chain extender (x3).
- Resin ( ⁇ 1) and the like it is preferable to include a urethane resin having a polyoxyalkylene skeleton as the urethane resin.
- polyol (x1) examples include polyol compounds such as alkylene diols, polyether type polyols, polyester type polyols, and polycarbonate type polyols, but are not particularly limited as long as they are polyols. May be a triol.
- diols are preferable from the viewpoints of availability, reactivity, and the like.
- diol examples include alkanediols such as 1,3-propanediol, 1,4-butanediol, 1,5-pentanediol, neopentyl glycol, 1,6-hexanediol, 1,7-heptanediol, and ethylene.
- alkylene glycols such as glycol, propylene glycol, diethylene glycol and dipropylene glycol, polyalkylene glycols such as polyethylene glycol, polypropylene glycol and polybutylene glycol, and polyoxyalkylene glycols such as polytetramethylene glycol.
- a glycol having a mass average molecular weight of 1000 to 3000 is preferable from the viewpoint of suppressing gelation in the reaction.
- polyvalent isocyanate compound (x2) examples include aromatic polyisocyanate, aliphatic polyisocyanate, and alicyclic polyisocyanate.
- aromatic polyisocyanate examples include 1,3-phenylene diisocyanate, 1,4-phenylene diisocyanate, 4,4′-diphenylmethane diisocyanate (MDI), 2,4-tolylene diisocyanate (2,4-TDI), 2 , 6-Tolylene diisocyanate (2,6-TDI), 4,4′-toluidine diisocyanate, 2,4,6-triisocyanate toluene, 1,3,5-triisocyanate benzene, dianisidine diisocyanate, 4,4 ′ -Diphenyl ether diisocyanate, 4,4 ', 4 "-triphenylmethane triisocyanate, 1,4-tetramethylxylylene diisocyanate, 1,3-tetramethylxylylene diis
- aliphatic polyisocyanate examples include trimethylene diisocyanate, tetramethylene diisocyanate, hexamethylene diisocyanate (HMDI), pentamethylene diisocyanate, 1,2-propylene diisocyanate, 2,3-butylene diisocyanate, 1,3-butylene diisocyanate, and dodeca.
- HMDI hexamethylene diisocyanate
- pentamethylene diisocyanate 1,2-propylene diisocyanate
- 2,3-butylene diisocyanate 1,3-butylene diisocyanate
- dodeca examples include methylene diisocyanate and 2,4,4-trimethylhexamethylene diisocyanate.
- Examples of the alicyclic polyisocyanate include 3-isocyanate methyl-3,5,5-trimethylcyclohexyl isocyanate (IPDI), 1,3-cyclopentane diisocyanate, 1,3-cyclohexane diisocyanate, 1,4-cyclohexane diisocyanate, Methyl-2,4-cyclohexane diisocyanate, methyl-2,6-cyclohexane diisocyanate, 4,4'-methylenebis (cyclohexyl isocyanate), 1,4-bis (isocyanatemethyl) cyclohexane, 1,4-bis (isocyanatemethyl) cyclohexane Etc.
- IPDI 3-isocyanate methyl-3,5,5-trimethylcyclohexyl isocyanate
- 1,3-cyclopentane diisocyanate 1,3-cyclohexane diisocyanate
- polyisocyanate compounds (x2) are a trimethylolpropane adduct type modified product of the above polyisocyanate, a burette type modified product reacted with water, and an isocyanurate type modified product containing an isocyanurate ring. Also good.
- polyvalent isocyanate compounds (x2) 4,4′-diphenylmethane diisocyanate (MDI) and 2,4-tolylene diisocyanate (2,4-TDI) are used from the viewpoint of obtaining a urethane-based polymer having excellent adhesive properties.
- 2,6-tolylene diisocyanate (2,6-TDI) hexamethylene diisocyanate (HMDI), 3-isocyanate methyl-3,5,5-trimethylcyclohexyl isocyanate (IPDI), and modified products thereof
- HMDI hexamethylene diisocyanate
- IPDI 3-isocyanate methyl-3,5,5-trimethylcyclohexyl isocyanate
- modified products thereof From the viewpoint of weather resistance, one or more selected from HMDI, IPDI, and modified products thereof are more preferable.
- chain extender (x3) a compound having at least one of at least one of a hydroxyl group and an amino group or a compound having at least three of at least one of a hydroxyl group and an amino group is preferable.
- the compound having at least one of a hydroxyl group and an amino group is preferably at least one compound selected from the group consisting of aliphatic diols, aliphatic diamines, alkanolamines, bisphenols, and aromatic diamines.
- aliphatic diol examples include alkanediols such as 1,3-propanediol, 1,4-butanediol, 1,5-pentanediol, neopentyl glycol, 1,6-hexanediol, and 1,7-heptanediol.
- alkylene glycols such as ethylene glycol, propylene glycol, diethylene glycol and dipropylene glycol.
- Examples of the aliphatic diamine include ethylenediamine, 1,3-propanediamine, 1,4-butanediamine, 1,5-pentanediamine, 1,6-hexanediamine, and the like.
- Examples of the alkanolamine include monoethanolamine, monopropanolamine, isopropanolamine and the like.
- Examples of bisphenol include bisphenol A and the like.
- Examples of the aromatic diamine include diphenylmethanediamine, tolylenediamine, xylylenediamine, and the like.
- Examples of the compound having at least three hydroxyl groups and amino groups include polyols such as trimethylolpropane, ditrimethylolpropane, pentaerythritol, dipentaerythritol, 1-amino-2,3-propanediol, and 1-methyl.
- Examples include amino alcohols such as amino-2,3-propanediol and N- (2-hydroxypropylethanolamine), and ethylene oxide or propylene oxide adducts of tetramethylxylylenediamine.
- the method for synthesizing the urethane-based prepolymer ( ⁇ 1) is not particularly limited.
- the polyol (x1) and the polyvalent isocyanate compound (x2), a catalyst added as necessary, and a solvent are charged into the reactor. And the like.
- the catalyst to be used is not particularly limited, and examples thereof include tertiary amine compounds and organometallic compounds.
- the molar ratio of NCO group to OH group ([NCO group] / [OH group]) is preferably 1.1 to 3.0, more preferably The reaction is preferably carried out so as to be 1.2 to 2.5.
- the isocyanate group content (NCO%) in the obtained urethane prepolymer ( ⁇ 1) is preferably 0.5 to 12% by mass, more preferably, as measured according to JIS K 1603-1. 1 to 4% by mass.
- the method for synthesizing the urethane polymer ( ⁇ 1) obtained by further subjecting the urethane prepolymer ( ⁇ 1) to a chain extension reaction using a chain extender (x3) is not particularly limited.
- the method is mentioned.
- a method in which a solution obtained by diluting a urethane prepolymer ( ⁇ 1) with a solvent is charged into a reactor, and a predetermined amount of a chain extender is charged into the reactor in a lump for reaction.
- a terminal terminator such as a compound having only one active hydrogen capable of reacting with an isocyanate group or a compound having only one amino group may be used.
- the compound having only one active hydrogen capable of reacting with an isocyanate group include monool compounds such as methanol and ethanol.
- the compound having only one amino group include diethylamine and morpholine.
- the resin composition forming the resin part (A) used in the present invention further contains a tackifier from the viewpoint of improving the adhesive strength of the sealing sheet. Can do.
- a specific tackifier the tackifier described with the resin composition which forms the resin part (B) mentioned later is mentioned.
- the softening point of the tackifier that can be used together with the resin composition forming the resin part (A) is preferably 60 to 170 ° C, more preferably 65 to 160 ° C, and still more preferably 70 to 150 ° C.
- the “softening point” is a value measured according to JIS K 2207.
- the resin composition forming the resin part (A) contains a resin having the above functional group such as an acrylic resin having the structural unit (p2) derived from the above functional group-containing monomer (p2)
- the resin composition forming the part (A) preferably further contains a crosslinking agent.
- a crosslinking agent reacts with the functional group of the said resin, and bridge
- crosslinking agent examples include: tolylene diisocyanate, hexamethylene diisocyanate, and the like, and isocyanate-based crosslinking agents such as adducts thereof; epoxy-based crosslinking agents such as ethylene glycol glycidyl ether; hexa [1- (2-methyl) -aziridinyl ] Aziridine type crosslinking agents such as triphosphatriazine; Chelate type crosslinking agents such as aluminum chelate; These crosslinking agents may be used alone or in combination of two or more. Among these, an isocyanate-based crosslinking agent is preferable from the viewpoints of increasing cohesion and improving interfacial adhesion, and availability.
- the amount of the crosslinking agent is appropriately adjusted depending on the number of functional groups in the resin structure contained in the resin composition forming the resin part (A). From the viewpoint of accelerating the crosslinking reaction, (meth) acrylic acid ester The amount is preferably 0.01 to 10 parts by mass, more preferably 0.03 to 7 parts by mass, and still more preferably 0.05 to 4 parts by mass with respect to 100 parts by mass of the resin having the above-described functional group such as a resin. .
- the resin composition forming the resin portion (A) may contain other additives depending on the use of the sealing sheet as long as the effects of the present invention are not impaired.
- other additives include ultraviolet absorbers, antioxidants, softeners (plasticizers), fillers, rust inhibitors, pigments, and dyes.
- the amount of the additives is preferably 0.01 to 6 parts by mass with respect to 100 parts by mass of the resin composition forming the resin part (A).
- the water vapor permeability measured in accordance with JIS K 7129 of the resin part (B) used in the present invention is 15 g / m 2 / day or less.
- the water vapor transmission rate of the resin composition forming the resin part (B) is preferably 14 g / m 2 / day or less, more preferably 13 g / m 2 / day or less, and further preferably 10 g / m 2.
- the value of the water vapor transmission rate means a value measured by the method described in the examples.
- the resin composition forming the resin part (B) used in the present invention is at least one selected from butyl rubber, polyisobutylene resin, styrene copolymer, polyisoprene resin, polybutadiene resin and polybutene resin. It is preferable that it is a resin composition containing resin. Among these, it is more preferable that polyisobutylene resin is included.
- Polyisobutylene resin The structure of the polyisobutylene resin is a resin having a polyisobutylene skeleton in the main chain or side chain, and a resin having the following structural unit (b).
- polyisobutylene resin examples include polyisobutylene, which is a homopolymer of isobutylene, a copolymer of isobutylene and isoprene, a copolymer of isobutylene and n-butene, a copolymer of isobutylene and butadiene, and a homopolymer of these.
- examples thereof include halogenated butyl rubber obtained by bromination or chlorination of a polymer or a copolymer. These resins may be used alone or in combination of two or more.
- the polyisobutylene resin is a copolymer, it is assumed that the constitutional unit composed of isobutylene is contained in the largest amount among all the monomer components.
- the thing containing the structural unit which becomes is preferable.
- the content of the structural unit composed of isobutylene is preferably 80 to 100% by mass, more preferably 90 to 100% by mass, and still more preferably 100% by mass with respect to all the structural units contained in the resin.
- Examples of the synthesis method of the polyisobutylene resin include a method of polymerizing a monomer component such as isobutylene in the presence of a Lewis acid catalyst such as aluminum chloride or boron trifluoride.
- a Lewis acid catalyst such as aluminum chloride or boron trifluoride.
- examples of commercially available products include Vistanex (manufactured by Exxon Chemical Co.), Hycar (manufactured by Goodrich), Opanol (manufactured by BASF), and the like.
- polyisobutylene resin (b-1) having a mass average molecular weight of 270,000 to 600,000
- polyisobutylene resin (b-1) a polyisobutylene resin having a mass average molecular weight of 270,000 to 600,000
- polyisobutylene resin (b-2) a polyisobutylene resin having a mass average molecular weight of 50,000 to 250,000
- polyisobutylene resin (b-2) having a mass average molecular weight of 50,000 to 250,000
- the polyisobutylene resin (b-1) is a polyisobutylene resin having a mass average molecular weight of 270,000 to 600,000.
- the polyisobutylene resin (b-1) having a specific mass average molecular weight By containing the polyisobutylene resin (b-1) having a specific mass average molecular weight, the durability and weather resistance of the sealing sheet can be improved, and the water vapor transmission rate can be lowered.
- the mass average molecular weight of the resin (b-1) is 270,000 to 600,000, preferably 270,000 to 480,000, more preferably from the viewpoint of improving the cohesive strength of the resin composition and reducing the water vapor transmission rate. It is 300,000 to 450,000, more preferably 320,000 to 400,000, and still more preferably 340,000 to 370,000. If the mass average molecular weight of the resin (b-1) is 270,000 or more, the cohesive strength of the resulting resin composition can be sufficiently improved, the adhesive strength of the sealing sheet using the resin composition, and moisture The effect of suppressing intrusion can be improved. Moreover, the concern about contamination of the adherend can be solved. Basically, the higher the mass average molecular weight, the lower the water vapor permeability and the better the holding power.
- the mass average molecular weight of the resin (b-1) is 600,000 or less, the cohesive force of the resulting resin composition becomes too high, and thus the adverse effects of flexibility and fluidity deterioration can be avoided.
- the wetting of the resin layer formed from the resin composition with the adherend can be improved.
- the solubility with respect to a solvent can be made favorable.
- the polyisobutylene resin (b-2) is a polyisobutylene resin having a mass average molecular weight of 50,000 to 250,000. By containing the polyisobutylene resin (b-2) having a specific mass average molecular weight, an excellent adhesive force can be imparted regardless of the type of adherend, and the balance between the adhesive force and the holding force is improved.
- the structure of the polyisobutylene resin (b-2) is a resin having a polyisobutylene skeleton in the main chain or side chain, as in the resin (b-1), and a resin having the structural unit (b). .
- the resin (b-2) examples include those exemplified for the above-mentioned resin (b-1). From the viewpoint of reducing the durability and weather resistance, and the water vapor transmission rate, the resin (b-2) is dense when polymerized. It preferably has a molecular structure and contains a structural unit composed of isobutylene that does not leave a polymerizable double bond in the main chain and side chain. The content of the structural unit composed of isobutylene is preferably 80 to 100% by mass, more preferably 90 to 100% by mass, and still more preferably 100% by mass with respect to all the structural units contained in the resin (b-2). is there.
- the resin (b-2) may be used alone or in combination of two or more.
- the synthetic method of the resin (b-2) and the commercially available products that can be used are the same as those of the resin (b-1).
- Resin (b-2) is well compatible with resin (b-1), and by appropriately plasticizing resin (b-1), the wettability with respect to the adherend is increased, and the adhesive physical properties and flexibility The holding power can be improved.
- the mass average molecular weight of the resin (b-2) is well compatible with the resin (b-1) and appropriately plasticizes the resin (b-1), and affects the other physical properties such as water vapor permeability. From the viewpoint of suppression, it is 50,000 to 250,000, preferably 100,000 to 250,000, more preferably 120,000 to 230,000, still more preferably 150,000 to 220,000, and still more preferably 180,000 to 210,000. .
- the resin (b-2) is 50,000 or more, in the resin layer formed from the resulting resin composition, the resin (b-2) is separated as a low molecular component and is deposited on the surface of the resin layer. It is possible to prevent the adverse effect of precipitation and contamination of the adherend. In addition, the influence on physical properties such as an increase in the amount of outgas generated at high temperatures can be avoided. On the other hand, if the mass average molecular weight of the resin (b-2) is 250,000 or less, the resin (b-2) can be sufficiently plasticized, and the resin layer formed from the resulting resin composition can be deposited. Wetting with the body can be improved.
- the content of the polyisobutylene-based resin (b-2) in the resin composition forming the resin part (B) is selected from the viewpoint of the balance between the adhesive force and holding power, and the effect of reducing the water vapor transmission rate.
- -1) 5 to 55 parts by mass with respect to 100 parts by mass, preferably 7 to 40 parts by mass, more preferably 8 to 30 parts by mass, and still more preferably 9 to 20 parts by mass.
- the content is 5 parts by mass or more, the resin (b-1) can be sufficiently plasticized, sufficiently wetted with the adherend, and excellent in adhesive strength.
- the content is 55 parts by mass or less, the cohesive force can be maintained without lowering the cohesive force and the holding force, and the durability against ultraviolet irradiation is also excellent.
- the resin composition for forming the resin part (B) is a polyisobutylene resin (b-3) (hereinafter referred to as a mass average molecular weight of 20,000 or more).
- Polyisobutylene resin (b-3)” or “resin (b-3)”) styrene-butadiene-styrene triblock copolymer (SBS), styrene- (ethylene-co-butylene)-
- SBS styrene-butadiene-styrene triblock copolymer
- SIB styrene-isobutylene diblock copolymers
- SIBS styrene-isobutylene-styrene triblock copolymers
- the polyisobutylene resin (b-3) is a polyisobutylene resin having a mass average molecular weight of 20,000 or more.
- the mass average molecular weight of the resin (b-3) is 20,000 or more, the cohesive force of the resin composition can be sufficiently obtained, and the adhesiveness can be sufficiently improved.
- the sealing sheet using a resin composition is used, the inhibitory effect of the moisture penetration
- the mass average molecular weight of the resin (b-3) is 20,000 or more, but preferably from 30,000 to 1,000,000, more preferably 5 from the above viewpoints and from the viewpoints of wettability to an adherend and solubility in a solvent. It is 10,000 to 800,000, more preferably 70,000 to 600,000, and still more preferably 140,000 to 450,000.
- the resin (b-3) from the viewpoint of improving the adhesive strength, durability, weather resistance, and wettability of the encapsulating sheet using the obtained resin composition, the above-mentioned polyisobutylene series having a high mass average molecular weight is used. It is preferable to use the resin (b-1) in combination with the polyisobutylene resin (b-2) having a low mass average molecular weight.
- the amount of the polyisobutylene resin relative to 100 parts by mass of the resin composition forming the resin part (B) of the present invention is preferably 20 to 95 from the viewpoint of improving the adhesive force and improving the effect of suppressing moisture intrusion.
- the mass is more preferably 25 to 90 parts by mass, still more preferably 30 to 85 parts by mass.
- the resin composition for forming the resin part (B) used in the present invention includes styrene-butadiene-styrene triblock copolymer (SBS), styrene- (ethylene-co-butylene) -styrene triblock copolymer (SEBS). ), At least one styrene copolymer (b-4) selected from styrene-isobutylene diblock copolymer (SIB) and styrene-isobutylene-styrene triblock copolymer (SIBS). .
- SIB styrene-isobutylene diblock copolymer
- SIBS styrene-isobutylene-styrene triblock copolymer
- the resin composition forming the resin part (B) contains at least one styrene copolymer selected from the above as the resin (b-4), thereby sealing using the resin composition While making the suppression effect of the water
- the resins (b-4) at least one selected from SBS and SEBS is preferable from the viewpoint of improving the adhesive strength of the sealing sheet using the resin composition.
- 1 or more types chosen from SIB and SIBS are preferable from a viewpoint of improving the suppression effect of the moisture permeation of the said sealing sheet.
- the mass average molecular weight (Mw) of the resin (b-4) is from the viewpoint of improving the adhesive effect of the sealing sheet while improving the moisture entry suppression effect of the sealing sheet using the obtained resin composition. It is preferably 10,000 to 400,000, more preferably 20,000 to 300,000, still more preferably 25,000 to 200,000, still more preferably 30,000 to 90,000. If the Mw of the component (b-4) is 10,000 or more, the adhesive strength of the sealing sheet using the obtained resin composition can be improved.
- the Mw of the component (b-4) is 400,000 or less, the resin layer formed from the obtained resin composition while maintaining good adhesive strength of the sealing sheet using the obtained resin composition The value of the water vapor transmission rate can be reduced, and the effect of suppressing the water entry of the sealing sheet can be improved.
- the softening point of the resin (b-4) is, from the viewpoint of improving the effect of suppressing moisture entry of the sealing sheet when the sealing sheet using the resin composition is used for sealing applications such as an organic EL element,
- the temperature is preferably 80 to 200 ° C, more preferably 90 to 160 ° C, still more preferably 100 to 140 ° C, and still more preferably 105 to 135 ° C.
- the ratio of styrene contained in the styrene copolymer of the resin (b-4) is preferably 5 to 50% by mass, more preferably 10 to 40% by mass, and further preferably 15 to 35% by mass.
- the content ratio [(b-3) / (b-4)] of the resin (b-3) to the resin (b-4) is preferably 40/60 to 95/5, more preferably 45/55 to 92/8, more preferably 50/50 to 90/10, even more preferably 55/45 to 88/12, still more preferably 60/40 to 85/15, and even more preferably 65/35 to 82/15 It is. If the content ratio is within the above range, the value of the water vapor permeability of the resin layer formed from the resin composition is improved while improving the adhesive strength of the sealing sheet using the obtained resin composition. It can be made small and the effect of suppressing the moisture intrusion of the sealing sheet can be made favorable.
- the content of the resin (b-4) with respect to the total amount of the resin composition forming the resin part (B) used in the present invention is preferably 2 to 60 from the viewpoint of improving the compatibility and the effect of suppressing moisture intrusion. It is preferably 4% to 55% by weight, more preferably 6% to 50% by weight, and still more preferably 8% to 47% by weight.
- the resin composition forming the resin portion (B) used in the present invention further contains a tackifier having a softening point of 135 ° C. or lower.
- the tackifier can be mixed with the resin composition forming the resin part (B) and other resin components, and has the function of improving the adhesion performance of these resin components, and the molecular weight of the oligomer region.
- Means a compound having The number average molecular weight of the tackifier is usually from 100 to 18000, preferably from 100 to 10,000.
- the softening point of the tackifier used in the present invention is preferably 135 ° C. or lower. It is preferable for the tackifier to have a softening point of 135 ° C. or lower because the adhesiveness of the resin composition containing the resin portion (B) can be prevented from significantly decreasing. Moreover, the zipping which generate
- the softening point of the tackifier is preferably 60 ° C. or higher, more preferably 70 ° C. or higher, from the viewpoint of improving the cohesive strength of the resulting resin composition and obtaining a resin composition that exhibits excellent tackiness. More preferably, it is 80 degreeC or more, More preferably, it is 90 degreeC or more.
- two or more tackifiers having different softening points may be combined. When using several tackifiers, the weighted average of the softening points of these tackifiers should just belong to the said range. Therefore, in the present invention, if the weighted average of the softening points of a plurality of tackifiers is 135 ° C.
- the tackifier having a softening point exceeding 135 ° C. is added to the resin part (B). You may contain in the resin composition which forms.
- the content of the tackifier having a softening point exceeding 135 ° C. is preferably 10% by mass or less, more preferably 4%, based on the total amount of the tackifier contained in the resin composition forming the resin part (B). It is at most mass%, more preferably at most 1 mass%, still more preferably at most 0.01 mass%.
- tackifiers include rosin resins such as aliphatic hydrocarbon resins, rosin resins, rosin phenol resins, and rosin ester resins; hydrogenated rosin resins obtained by hydrogenating these rosin resins; Terpene resins such as resins, terpene phenolic resins, aromatic modified terpene resins; hydrogenated terpene resins obtained by hydrogenating these terpene resins; C5 petroleum resins and the C5 petroleum Hydrogenated petroleum resin of resin; C9 petroleum resin obtained by copolymerizing C9 fraction and hydrogenated petroleum resin of this C9 petroleum resin; The following are mentioned. You may use the said tackifier individually or in combination of 2 or more types.
- C5 fraction means an unsaturated hydrocarbon having 5 carbon atoms, such as pentene, isoprene, piperine, 1.3-pentadiene, which is produced by the thermal decomposition of petroleum naphtha.
- Petroleum resin means a resin obtained by copolymerizing this C5 fraction and containing the C5 fraction as a main component (including at least 20% by mass or more).
- C9 fraction means an unsaturated hydrocarbon having 9 carbon atoms such as indene, vinyltoluene, ⁇ or ⁇ -methylstyrene, which is generated by thermal decomposition of petroleum naphtha.
- Resin means a resin obtained by copolymerizing the C9 fraction and containing the C9 fraction as a main component (including at least 20% by mass or more).
- the above-mentioned “hydrogenated resin” includes not only a completely hydrogenated resin but also a partially hydrogenated resin partially hydrogenated.
- the content of the tackifier is preferably 5 to 60 parts by mass, more preferably 8 to 50 parts by mass, and still more preferably 10 to 100 parts by mass with respect to a total of 100 parts by mass of the resin composition forming the resin part (B).
- the amount is 45 parts by mass, more preferably 15 to 42 parts by mass.
- the resin layer formed from the obtained resin composition can exhibit an excellent adhesive force regardless of the adherend, Occurrence can be suppressed. Moreover, the value of the water-vapor-permeability of the said resin layer is small, and the sealing sheet excellent in the suppression effect of moisture permeation can be obtained.
- the resin composition forming the resin part (B) of the present invention may further contain other additives as long as the effects of the present invention are not impaired.
- examples of other additives include other additives described in the resin composition forming the above-described resin portion (A).
- Other additives may be used alone or in combination of two or more.
- ⁇ Support> As a support body, if it is a sheet
- various types of paper such as high-quality paper, art paper, coated paper, glassine paper, laminated paper obtained by laminating a thermoplastic resin such as polyethylene on these paper base materials, various synthetic papers, aluminum foil, copper foil and iron Metal foil such as foil, porous material such as nonwoven fabric, polyolefin resin such as polyethylene resin and polypropylene resin, polyester resin such as polybutylene terephthalate resin and polyethylene terephthalate resin, acetate resin, ABS resin, polystyrene resin, vinyl chloride resin, etc.
- a sheet-shaped substrate such as a plastic film or sheet may be unstretched, or may be stretched in a uniaxial direction or a biaxial direction such as longitudinal or lateral.
- the support used may or may not be colored, but since it is used as a sealing member, it is preferably one that sufficiently transmits ultraviolet rays, and more preferably colorless and transparent in the visible light region.
- the thickness of the support is not particularly limited, but is preferably 10 to 250 ⁇ m, more preferably 15 to 200 ⁇ m, and still more preferably 20 to 150 ⁇ m from the viewpoint of ease of handling.
- the support may further contain an ultraviolet absorber, a light stabilizer, an antioxidant, an antistatic agent, a slip agent, an antiblocking agent, a colorant and the like.
- the support is a plastic material
- a surface treatment such as an oxidation method or a concavo-convex method as necessary from the viewpoint of improving the adhesion between the support and the resin layer.
- the oxidation method is not particularly limited, and examples thereof include a corona discharge treatment method, a plasma treatment method, chromic acid oxidation (wet), flame treatment, hot air treatment, and ozone / ultraviolet irradiation treatment.
- it does not specifically limit as an uneven
- These surface treatments are appropriately selected depending on the type of the support, but the corona discharge treatment method is preferred from the viewpoint of improving the adhesion with the resin layer and operability.
- primer treatment can also be performed.
- a sealing layer may be provided between the support and the resin layer as desired.
- this sealing layer is used to further improve the adhesion between the support and the resin layer, or when the support is too flexible. Is provided to provide rigidity.
- Such a sealing layer is not particularly limited, but for example, a styrene-butadiene copolymer, an acrylic resin, a polyester resin, a polyurethane resin, a polystyrene resin, or the like as a main component (containing at least 20% by mass or more) And a layer made of a material added with a filler such as clay, silica, calcium carbonate, titanium oxide, and zinc oxide as necessary.
- the thickness of the sealing layer is not particularly limited, but is usually 0.1 to 30 ⁇ m.
- Gas barrier film As the support of the sealing sheet of the present invention, it is preferable to use a gas barrier film having a gas barrier substrate and a gas barrier layer.
- the said gas barrier film should just have a gas barrier layer in the at least one surface side of the base material for gas barrier films.
- a gas barrier film has a single layer or multiple layers of gas barrier layer which consists of 1 or more types chosen from an inorganic layer, an organic layer, and a metal layer.
- the base material for the gas barrier film is not particularly limited.
- polyolefin such as polyethylene and polypropylene
- polyester such as polyethylene terephthalate and polybutylene terephthalate
- polyimide polyamideimide
- wholly aromatic polyamide nylon 6, nylon 66
- nylon Polyphenylene such as polymer, lubornene polymer, monocyclic olefin polymer, cyclic conjugated diene polymer, vinyl alicyclic hydrocarbon polymer, and cycloolefin polymers such as hydrides thereof, polyphenylene, etc.
- Examples thereof include a sheet made of a resin of ether, polyether ketone, polyether ether ketone, polycarbonate, polysulfone, polyether sulfone, polyphenylene sulfide, or polyarylate.
- polyester, polyamide or cycloolefin polymer is preferable, and polyester or cycloolefin polymer is more preferable from the viewpoint of excellent transparency and versatility.
- the thickness of the gas barrier film substrate is not particularly limited, but is preferably 2 to 200 ⁇ m, more preferably 10 to 150 ⁇ m, and still more preferably 20 to 100 ⁇ m from the viewpoint of ease of handling.
- the material for forming the gas barrier layer is not particularly limited as long as it prevents the permeation of oxygen and water vapor, but when the gas barrier layer has an inorganic layer, the inorganic layer includes diamond-like glass, diamond-like carbon, It is preferably formed from an inorganic material containing one or more selected from silicon oxide, silicon nitride, and silicon carbide.
- the organic layer is formed from an organic material containing at least one selected from polyimide, polyamide, polyamideimide, polyphenylene ether, polyetherketone and polyetheretherketone. It is preferable.
- the gas barrier property may be improved by performing surface modification such as plasma ion implantation treatment or vacuum ultraviolet irradiation treatment on the inorganic layer or the organic layer formed on the base material for the gas barrier film.
- the metal layer is preferably formed from one or more selected from aluminum, copper, tin and zinc.
- the method for forming the gas barrier layer may be appropriately selected according to the material to be used.
- the gas barrier layer material is formed on a gas barrier film substrate by vapor deposition, sputtering, ion plating, thermal CVD, plasma CVD, or the like, or the gas barrier layer material is an organic solvent. Examples include a method of applying the dissolved solution to the base material for gas barrier film.
- the thickness of the gas barrier layer is preferably 10 to 2000 nm, more preferably 50 to 500 nm.
- an anchor layer is preferably provided on the substrate, and the thickness of the anchor layer is preferably 1 to 2000 nm, more preferably 1 ⁇ 1000 nm.
- the material constituting the anchor layer include acrylic resin and polyester resin.
- a release sheet that has been subjected to a double-sided release process, a release sheet that has been subjected to a single-sided release process, or the like is used.
- Examples include a release sheet coated on a release sheet substrate.
- the base material for the release sheet include paper base materials such as glassine paper, coated paper, and high-quality paper, laminated paper obtained by laminating a thermoplastic resin such as polyethylene on these paper base materials, or polyethylene terephthalate resin, polybutylene.
- polyester resin films such as terephthalate resin and polyethylene naphthalate resin
- plastic films such as polyolefin resin films such as polypropylene resin and polyethylene resin.
- the release agent examples include rubber elastomers such as silicone resins, olefin resins, isoprene resins, and butadiene resins, long chain alkyl resins, alkyd resins, and fluorine resins.
- the thickness of the release sheet is not particularly limited, but is preferably 20 to 200 ⁇ m, more preferably 25 to 150 ⁇ m.
- ⁇ Manufacturing method of sealing sheet> There is no restriction
- the resin composition forming the resin part (A) used in the present invention and the resin composition forming the resin part (B) are, for example, methyl ethyl ketone, acetone, ethyl acetate, tetrahydrofuran, dioxane, cyclohexane, n-hexane, toluene Alternatively, an organic solvent such as xylene, n-propanol, or isopropanol may be blended to form a solution of the resin composition.
- the solid content concentration of the resin composition solution that forms the resin part (A) and the solid content concentration of the resin composition solution that forms the resin part (B) are preferably 10 respectively.
- the solid content concentration is 10% by mass or more, the amount of the organic solvent used is sufficient, and if it is 60% by mass or less, the viscosity becomes moderate and a solution having excellent coating workability can be obtained.
- Examples of the coating method include screen printing, spin coating, spray coating, bar coating, knife coating, roll coating, roll knife coating, blade coating, die coating, and gravure coating. .
- the encapsulating sheet of the present invention has excellent interfacial adhesion and interfacial adhesion with an adherend, and is particularly excellent in the effect of suppressing moisture intrusion. Therefore, the sealing sheet of the present invention is suitable as a sealing member for an organic EL element or the like, and when the sealing sheet of the present invention is used as a sealing member, moisture intrusion or driving of the organic EL element can be performed. Decrease in adhesion between the sealing sheet substrate (adhered body) and the sealing sheet due to heat generation can be suppressed, and deterioration of characteristics of the organic EL element can be suppressed.
- the encapsulating sheet of the present invention is, for example, an organic device such as an organic transistor, an organic memory, or an organic EL element; a liquid crystal display; an electronic paper; a thin film transistor; an electrochromic device; A thermoelectric conversion device; a piezoelectric conversion device; an electricity storage device; and the like.
- the sealing sheet of this invention is used as a sealing use of an organic EL element.
- the sealing structure of this invention is a sealing structure formed by sealing the to-be-sealed body provided on the board
- An example of the sealing structure according to the embodiment of the sealing structure sealed with the sealing sheet of the present invention will be described with reference to FIG. 3 and FIG. 4. As long as the above effects are exhibited, the present invention is not limited to the following examples. 3 and 4 are plan views showing a part of the sealing structure in which the support 5 and the substrate (adhered body) 9 are omitted for the sake of explanation.
- the sealing structure 301 (a) includes the resin portion (A) 1 at the outer edge portion of the resin portion (B) 2 and the resin portion (A) 1. Forms a closed region 3, and the resin portion (B) 2 exists in the closed region 3.
- the sealed object 7 is arranged in the closed region 3.
- FIG. 3B shows an example that the cross-sectional view on XX ′ in FIG.
- the sealing structure 301 (b) is a structure in which the sealing sheet 8 including the resin layer 4 and the support 5 is provided on the substrate (adhered body) 9.
- An object to be sealed 7 is arranged on a substrate (adhered body) 9, and resin parts (A) 1 exist at both ends of the resin part (B) 2 that seals the object 7 to be sealed.
- the resin portion (A) 1 is in contact with both the substrate (adhered body) 9 and the support 5.
- one mode shown in the cross-sectional view of FIG. 3C shows an example that the cross-sectional view on XX ′ in FIG.
- the sealing structure 301 (c) is a structure in which a sealing sheet 8 including the resin layer 4 and the support 5 is provided on a substrate (adhered body) 9.
- An object to be sealed 7 is arranged on a substrate (adhered body) 9, and resin parts (A) 1 exist at both ends of the resin part (B) 2 that seals the object 7 to be sealed.
- the resin portion (A) 1 is in contact only with the substrate (adhered body) 9. Only the resin portion (B) 2 that seals the object 7 is in contact with the support 5 side.
- the resin layer 302 (a) of the sealing structure is provided with the sealing sheet 8 including the resin layer 4 and the support 5 on the substrate (adhered body) 9.
- the resin portion (A) 1 and the resin portion (B) 2 are arranged in a lattice shape, the resin portion (A) 1 forms a closed region 3, and the resin portion is in the closed region 3. (B) 2 exists.
- the sealed object 7 is arranged in the closed region 3.
- FIG. 4B shows an example that the cross-sectional view on XX ′ in FIG. 4A can take. In the cross-sectional view of FIG.
- the sealing structure 302 (b) is a structure in which a sealing sheet 8 including a resin layer 4 and a support 5 is provided on a substrate (adhered body) 9.
- An object to be sealed 7 is arranged on a substrate (adhered body) 9, the object to be sealed 7 is sealed by the resin portion (B) 2, and the substrate (adhered body) 9 is sealed to the object 7 to be sealed.
- the resin part (B) 2, the resin part (A) 1, and the resin part (B) are arranged on a straight line from the outer edge part of the object 7 to be sealed to the outer edge part of the substrate (adhered body) 9. 2) exist in this order.
- the resin portion (A) 1 is in contact with both the substrate (adhered body) 9 and the support 5.
- the sealing structure 302 (c) is a structure in which a sealing sheet 8 composed of the resin layer 4 and the support 5 is provided on a substrate (adhered body) 9.
- An object to be sealed 7 is arranged on a substrate (adhered body) 9, the object to be sealed 7 is sealed by the resin portion (B) 2, and the substrate (adhered body) 9 is sealed to the object 7 to be sealed.
- the resin part (B) 2, the resin part (A) 1, and the resin part (B) are arranged on a straight line from the outer edge part of the object 7 to be sealed to the outer edge part of the substrate (adhered body) 9. 2) exist in this order.
- the resin portion (A) 1 is in contact only with the substrate (adhered body) 9. Only the resin portion (B) 2 that seals the object 7 is in contact with the support 5 side.
- the object 7 to be sealed is placed on the substrate (adhered body) 9 on the opposite side to the support 5, so that the resin portion (A) 1 and the resin part (B) 2 are present on the substrate (adhered body) 9 side, so that the resin part (A) 1 and the resin part (B) 2 and the substrate (adhered body) 9 in particular.
- the lowering of the adhesion is suppressed and the interfacial adhesion is further improved, so that it is possible to effectively prevent moisture from entering between the substrate (adhered body) 9 and the resin layer 4, A sealed structure having excellent durability under warming and humidification can be obtained.
- a glass plate or a gas barrier film is used as the substrate (adhered body) included in the sealing structure of the present invention.
- the glass plate those conventionally used for electronic devices can be used.
- the gas barrier film the same film as the gas barrier film described above for the sealing sheet can be used.
- the thickness of the substrate (adherent) is preferably 1 to 300 ⁇ m, more preferably 20 to 200 ⁇ m.
- the substrate (adherent) has a water vapor transmission rate of less than 0.1 g / m 2 / day measured at 40 ° C. and 90% RH (relative humidity) as measured in accordance with JIS K 7129.
- substrate adherence body
- the gas-permeation rate measuring apparatus as described in the Example mentioned later.
- the object to be sealed to be sealed by the sealing structure of the present invention is preferably an organic EL element or the like as described above for the sealing sheet.
- the sealing structure of the present invention it is possible to suppress a decrease in the adhesion between the sealing sheet and the substrate (adhered body) due to moisture intrusion or heat generation during driving of the organic EL element, thereby reducing the characteristic deterioration of the organic EL element. Can be suppressed.
- the object to be sealed is an organic EL display element, a liquid crystal display element, or a solar cell element because the effect of the sealing structure of the present invention is more exhibited.
- the light emitting device, the display device, or the solar cell having the sealing sheet or the sealing structure according to the present invention is reduced in adhesion between the sealing sheet and the substrate (adhered body) due to moisture intrusion or heat generation during driving of each element. Can be suppressed, and deterioration of characteristics of each element can be suppressed, so that durability under heating and humidification conditions is excellent.
- the adhesiveness between the sealing sheet and the substrate (adhered body) is reduced due to moisture intrusion or heat generation during driving of the organic EL element.
- a liquid crystal display and a solar cell having the sealing sheet or the sealing structure of the present invention are also excellent in durability under heating and humidification conditions.
- the mass average molecular weight (Mw) and softening point of each component used in the following Examples and Comparative Examples are values measured by the following methods.
- the release surface of a polyethylene terephthalate film (product name “SP-PET381130”, manufactured by Lintec Corporation, thickness 38 ⁇ m) whose surface was subjected to silicone release treatment was attached to the formed resin layer surface as a light release film.
- a polyethylene terephthalate film (Mitsubishi Resin Co., Ltd., thickness 6 ⁇ m) was laminated and sandwiched between the two polyethylene terephthalate films. It was set as the sample for water-vapor-permeation rate measurement which consists of a resin layer.
- the measurement of water vapor transmission rate is based on JIS K 7129, using a transmission meter (product name “L89-500” manufactured by LYSSY) in an environment of 40 ° C. and 90% RH (relative humidity). did.
- the water vapor transmission rate of the polyethylene terephthalate film used for the lamination was 43 g / m 2 / day. That is, if the water vapor barrier property of the resin layer is completely zero, a value of around 43 g / m 2 / day is shown. The lower the value, the better the water vapor barrier property of the resin layer.
- Example 1 According to the prescription in Table 1, a toluene solution of the resin composition used for the resin part (A) obtained in Production Example 1 and a toluene solution of the resin composition used for the resin part (B) were prepared. Each solution was dried on a release film surface of a heavy release film (product name “SP-PET38T103-1”, manufactured by Lintec Corporation, cut into 240 mm ⁇ 240 mm) with a screen printer so that the thickness after drying was 50 ⁇ m. In the shape shown in the grid pattern (FIG. 1A), the resin part (A) is applied so that the line width is 20 mm, and dried at 100 ° C. for 2 minutes to form the resin part (A) of the resin layer. did.
- a heavy release film product name “SP-PET38T103-1”, manufactured by Lintec Corporation, cut into 240 mm ⁇ 240 mm
- the resin part (B) of the resin layer was formed by applying the resin part (B) in the central part so that one side was 100 mm and drying at 100 ° C. for 2 minutes. In that case, it apply
- the gas barrier film used here was produced by the following method.
- the supporting substrate is provided with an anchor layer made of an acrylic resin having a thickness of 100 nm on one surface of a polyester film having a thickness of 100 ⁇ m, and then an inorganic layer made of a silicon oxide having a thickness of 100 nm is formed on the anchor layer.
- the provided gas barrier film was used.
- an anode, a hole transport layer, a light emitting layer, and a cathode are sequentially formed on a glass plate (arithmetic average roughness Ra: 2 nm, maximum protrusion height Rp: 18 nm) as a substrate (adherent).
- An organic EL display element (sealed object) having a structure of anode / hole transport layer / light emitting layer / cathode was provided. This anode was formed by patterning by etching after ITO was formed by sputtering.
- the hole transport layer was formed by vapor deposition using ⁇ -naphthylphenyldiamine.
- the light emitting layer was formed using tris (8-quinolinol) aluminum.
- a cathode having a two-layer structure was formed by vapor deposition using calcium and silver. Then, the resin layer exposed by peeling and removing the heavy release sheet of the sealing sheet laminated with the prepared gas barrier film is attached at room temperature so that the object to be sealed on the prepared substrate (adhered body) is sealed.
- the sealing structure was produced by attaching.
- Example 2 In Example 1, instead of applying in a grid pattern, the same method as in Example 1 was applied except that the resin part (B) was applied so that the line width was 20 mm in the shape shown in FIG. Thus, a sealing structure was produced. In addition, it apply
- Example 3 In Example 1, instead of applying in a grid pattern, the same method as in Example 1 was applied except that the resin part (A) was applied so that the line width was 20 mm in the shape shown in FIG. Thus, a sealing structure was produced. In addition, it apply
- Example 4 A sealing structure was produced in the same manner as in Example 1 except that the formulation of the resin composition used for the resin part (B) shown in Table 1 was used.
- Example 5 A sealing structure was produced in the same manner as in Example 1 except that the formulation of the resin composition used for the resin part (B) shown in Table 1 was used.
- Comparative Example 2 Comparative Example, except that the resin composition used for the resin part (B) obtained in Production Example 1 was not used and only the resin composition used for the resin part (A) shown in Table 1 was applied to form a resin layer. A sealing structure was produced in the same manner as in Example 1.
- the sealing structures produced in the examples and comparative examples described in Table 1 were used for 4 weeks and 8 weeks in a constant temperature and humidity chamber set at 40 ° C. and 90% RH (relative humidity). Stored at and taken out. About the taken-out sealing structure, drive conditions were 10 mA / cm ⁇ 2 >, the sealing structure was made to light-emit, and the light emission part was observed by 25 times using the stereomicroscope, and the presence or absence of the dark spot was observed. The sealing ability was evaluated according to the following criteria. A: The number of dark spots is zero. -B: The number of dark spots is 1 to 3. C: The number of dark spots is 4 or more.
- the sealing sheet of the present invention when the sealing structure is produced, in addition to the effect of preventing moisture intrusion due to the low water vapor permeability of the sealing sheet itself, Moisture that enters the sealing structure from the inside can also be prevented, so that the sealing structure sealed with the sealing sheet and the device having the sealing sheet or the sealing structure are not suitable. Excellent durability under warm and humid conditions. Therefore, the sealing sheet of this invention is used suitably, for example for sealing an organic EL element, a liquid crystal display element, or a solar cell element. Furthermore, for example, the sealing sheet or the sealing structure and the sealing sheet are also suitably used in a device such as a light-emitting device, a display device, or a solar cell having the element.
- Resin part (A) 2 Resin part (B) 3 Closed region 4 Resin layer 5 Support 6 Release sheet 7 Sealed object 8 Sealing sheet 9 Substrate (adhered body) 101 to 106 Resin layer surface 201 to 204 of sealing sheet Cross section 301 (a) of sealing sheet Plane 301 (b) and 301 (c) of sealing structure 302 (a) Sealing structure Body plane 302 (b), 302 (c) Cross-section of the sealing structure
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Abstract
Description
[1]アクリル系樹脂及びウレタン系樹脂から選ばれる1種以上の樹脂を含む樹脂組成物より形成されてなる樹脂部分(A)と、JIS K 7129に準拠して測定した水蒸気透過率が15g/m2/day以下となる樹脂部分(B)とを含む樹脂層を有する封止シートであって、前記樹脂層の少なくとも一方の表面上に、樹脂部分(A)と樹脂部分(B)とが存在している、封止シート。
[2]樹脂層の少なくとも一方の表面上に、樹脂部分(A)又は樹脂部分(B)が閉じた領域を形成し、当該閉じた領域内に他方の樹脂部分が存在してなる、上記[1]に記載の封止シート。
[3]樹脂層の少なくとも一方の表面上で、樹脂部分(A)の合計表面積と樹脂部分(B)の合計表面積との比率〔(A)面積/(B)面積〕が10/90~90/10である、上記[1]又は[2]に記載の封止シート。
[4]支持体上に、前記樹脂層を有する、上記[1]~[3]のいずれかに記載の封止シート。
[5]樹脂層の支持体側の表面上には樹脂部分(B)のみが存在し、前記樹脂層の他方の表面上には樹脂部分(A)及び樹脂部分(B)が存在している、上記[4]に記載の封止シート。
[6]支持体が、ガスバリアフィルムである、上記[4]又は[5]に記載の封止シート。
[7]樹脂部分(B)を形成する樹脂組成物が、ブチルゴム、ポリイソブチレン系樹脂、スチレン系共重合体、ポリイソプレン系樹脂、ポリブタジエン系樹脂及びポリブテン系樹脂から選ばれる1種以上の樹脂を含む、上記[1]~[6]のいずれかに記載の封止シート。
[8]樹脂部分(B)を形成する樹脂組成物が、質量平均分子量27万~60万のポリイソブチレン系樹脂(b-1)、及び質量平均分子量5万~25万のポリイソブチレン系樹脂(b-2)を含む、上記[7]に記載の封止シート。
[9]樹脂部分(B)を形成する樹脂組成物が、質量平均分子量が2万以上のポリイソブチレン系樹脂(b-3)、並びにスチレン-ブタジエン-スチレントリブロック共重合体(SBS)、スチレン-(エチレン-co-ブチレン)-スチレントリブロック共重合体(SEBS)、スチレン-イソブチレンジブロック共重合体(SIB)、及びスチレン-イソブチレン-スチレントリブロック共重合体(SIBS)から選ばれる1種以上のスチレン系共重合体(b-4)を含む、上記[7]に記載の封止シート。
[10]スチレン系共重合体(b-4)の軟化点が、80~200℃である、上記[9]に記載の封止シート。
[11]樹脂部分(B)を形成する樹脂組成物が、更に、軟化点が135℃以下の粘着付与剤を含む、上記[1]~[10]のいずれかに記載の封止シート。
[12]有機EL素子の封止用として用いられる、上記[1]~[11]のいずれかに記載の封止シート。
[13]基板(被着体)上に設けられた被封止物を上記[1]~[12]のいずれかに記載の封止シートにより封止してなる、封止構造体。
[14]被封止物が、前記封止シートの表面上で樹脂部分(B)により閉じた領域内に位置する、上記[13]に記載の封止構造体。
[15]被封止物が、有機EL素子、有機ELディスプレイ素子、液晶ディスプレイ素子、又は太陽電池素子である、上記[13]又は[14]に記載の封止構造体。
[16]基板(被着体)が、ガラス板又はガスバリアフィルムである上記[13]~[15]のいずれかに記載の封止構造体。
[17]上記[1]~[12]のいずれかに記載の封止シート、又は上記[13]~[16]のいずれかに記載の封止構造体を有する、発光装置、表示装置又は太陽電池。
本発明の封止シートは、アクリル系樹脂及びウレタン系樹脂から選ばれる1種以上の樹脂を含む樹脂組成物より形成されてなる樹脂部分(A)と、JIS K 7129に準拠して測定した水蒸気透過率が15g/m2/day以下となる樹脂部分(B)とを含む樹脂層を有する封止シートであって、前記樹脂層の少なくとも一方の表面上に、樹脂部分(A)と樹脂部分(B)とが存在している構成を有する。
当該構成を有する本発明の封止シートを用いた場合、低水蒸気透過率である樹脂部分(B)による封止シート全体の水分浸入抑制効果に加えて、更に、基板(被着体)との界面密着性が良好な樹脂部分(A)によって、封止シートと基板(被着体)との間から浸入し得る水分を効果的に抑制することができ、該封止シートを有する封止構造体及び装置の加温・加湿下での耐久性を向上できる。
樹脂層の少なくとも一方の表面上は、例えば、図1(a)~(f)に示すような形状を有する。
図1(a)~(f)に示すように、封止シートの樹脂層の少なくとも一方の表面上には、樹脂部分(A)1と樹脂部分(B)2とが存在している。
図1(a)に示す構成において、封止シートの樹脂層の表面101は、樹脂部分(A)1と樹脂部分(B)2とが格子状に配置されており、樹脂部分(A)1が閉じた領域3を形成し、当該閉じた領域3内に樹脂部分(B)2が形成されている。
図1(b)に示す構成において、封止シートの樹脂層の表面102は、樹脂部分(A)1の外縁部に樹脂部分(B)2が配置されており、樹脂部分(B)2が閉じた領域3を形成し、当該閉じた領域3内に樹脂部分(A)1が配置されている。
図1(c)に示す構成において、封止シートの樹脂層の表面103は、樹脂部分(B)2の外縁部に樹脂部分(A)1が配置されており、樹脂部分(A)1が閉じた領域3を形成し、当該閉じた領域3内に樹脂部分(B)2が配置されている。
図1(d)に示す構成において、封止シートの樹脂層の表面104は、樹脂部分(A)1中に樹脂部分(B)2が円状に配置されており、樹脂部分(B)2が閉じた領域3を形成し、当該閉じた領域3内に樹脂部分(A)1が配置されている。
図1(e)に示す構成において、封止シートの樹脂層の表面105は、十分な界面密着性を確保できるように各樹脂部分(A)1が封止シートの外縁部に断続的に配置され、各樹脂部分(A)1以外の部分には樹脂部分(B)2が配置されている。
図1(f)に示す構成において、封止シートの樹脂層の表面106は、十分な界面密着性を確保できるように各樹脂部分(A)1の少なくとも1辺が封止シートの外縁部に接するように配置され、各樹脂部分(A)1以外の部分には樹脂部分(B)2が配置されている。
なお、図1(e)及び(f)に示す構成でもよいが、基板(被着体)と封止シートとの界面密着性を向上させて封止シートの水分浸入抑制効果を向上できる観点から、図1(a)~(d)に示すように、樹脂層の少なくとも一方の表面において、樹脂部分(A)1又は樹脂部分(B)2が閉じた領域3を形成し、当該閉じた領域には他方の樹脂部分が存在している構成であることが好ましい。また、図1(a)及び図1(d)において、樹脂部分(A)1と樹脂部分(B)2とが逆に配置されている構成であってもよい。
本発明の封止シートの構成としては、例えば、図2(a)及び(b)に示すように、支持体5上に樹脂層4を有する構成の封止シート201及び202が挙げられる。また、図2(c)に示すように、支持体5、樹脂層4、及び剥離シート6をこの順で積層した構成の封止シート203、及び、図2(d)に示すように、2枚の剥離シート6で樹脂層4を挟持した構成の封止シート204が挙げられる。
また、前記樹脂層4は、図2(a)~(c)に示すように、支持体5上に設けられることが好ましい。また、図2(b)に示すように、前記支持体5側の前記樹脂層4の表面上には樹脂部分(B)2のみが存在し、他方の表面上には樹脂部分(A)1及び樹脂部分(B)2が存在している樹脂層4であってもよい。
以下、本発明の封止シートに含まれる成分について順次説明する。
本発明で使用する樹脂部分(A)を形成する樹脂組成物は、アクリル系樹脂及びウレタン系樹脂から選ばれる1種以上を含む。
本発明で用いるアクリル系樹脂は、アルキル(メタ)アクリレート由来の構成単位を含むアクリル系樹脂が挙げられるが、炭素数4以上のアルキル(メタ)アクリレート(以下、「モノマー(p1)」ともいう)由来の構成単位(p1)を含むアクリル系樹脂であることが好ましい。
モノマー(p1)が有するアルキル基の炭素数としては、封止シートの界面密着力を向上させる観点から、好ましくは4~20、より好ましくは4~12、更に好ましくは4~6である。また、モノマー(p1)のアルキル基は、直鎖及び分岐鎖のいずれであってもよい。
なお、これらのモノマー(p1)は、単独で又は2種以上組み合わせて用いてもよい。
これらの中でも、封止シートの界面密着力を向上させる観点から、ブチル(メタ)アクリレートが好ましく、n-ブチル(メタ)アクリレートがより好ましい。
なお、ここでいう、「官能基含有モノマー(p2)」の「官能基」とは、後述の架橋剤と反応し、架橋起点となり得る官能基又は架橋促進効果を有する官能基を意味する。
これらの中でも、水酸基含有モノマー、カルボキシ基含有モノマーが好ましい。
その他のモノマーとしては、アクリル系モノマーと共重合可能なモノマーから選択することができ、例えば、メチル(メタ)アクリレート、エチル(メタ)アクリレート、プロピル(メタ)アクリレート等の炭素数1~3のアルキル基を有するアルキル(メタ)アクリレートモノマー、スチレン、α-メチルスチレン、ビニルトルエン、蟻酸ビニル、酢酸ビニル、アクリロニトリル、アクリルアミド等のモノマー(p2)として挙げたもの以外のビニル系モノマー等が挙げられる。
本発明で用いるウレタン系樹脂としては、主鎖及び/又は側鎖に、ウレタン結合及び尿素結合の少なくとも一方を有する重合体であれば、特に制限されず、例えば、ポリオール(x1)と多価イソシアネート化合物(x2)とを反応して得られるウレタン系プレポリマー(α1)や、当該ウレタン系プレポリマー(α1)に対して、更に鎖延長剤(x3)を用いた鎖延長反応を行い得られるウレタン系樹脂(β1)等が挙げられる。
これらの中でも、ウレタン系樹脂として、ポリオキシアルキレン骨格を有するウレタン系樹脂を含むことが好ましい。
なお、本発明において、ウレタン系樹脂は、単独で又は2種以上を組み合わせて用いてもよい。
これらのジオールの中でも、さらに鎖延長剤(x3)との反応を行う場合、当該反応においてゲル化を抑制する観点から、質量平均分子量1000~3000のグリコールが好ましい。
芳香族ポリイソシアネートとしては、例えば、1,3-フェニレンジイソシアネート、1,4-フェニレンジイソシアネート、4,4’-ジフェニルメタンジイソシアネート(MDI)、2,4-トリレンジイソシアネート(2,4-TDI)、2,6-トリレンジイソシアネート(2,6-TDI)、4,4’-トルイジンジイソシアネート、2,4,6-トリイソシアネートトルエン、1,3,5-トリイソシアネートベンゼン、ジアニシジンジイソシアネート、4,4’-ジフェニルエーテルジイソシアネート、4,4’,4”-トリフェニルメタントリイソシアネート、1,4-テトラメチルキシリレンジイソシアネート、1,3-テトラメチルキシリレンジイソシアネート等が挙げられる。
脂肪族ポリイソシアネートとしては、例えば、トリメチレンジイソシアネート、テトラメチレンジイソシアネート、ヘキサメチレンジイソシアネート(HMDI)、ペンタメチレンジイソシアネート、1,2-プロピレンジイソシアネート、2,3-ブチレンジイソシアネート、1,3-ブチレンジイソシアネート、ドデカメチレンジイソシアネート、2,4,4-トリメチルヘキサメチレンジイソシアネート等が挙げられる。
脂環式ポリイソシアネートとしては、例えば、3-イソシアネートメチル-3,5,5-トリメチルシクロヘキシルイソシアネート(IPDI)、1,3-シクロペンタンジイソシアネート、1,3-シクロヘキサンジイソシアネート、1,4-シクロヘキサンジイソシアネート、メチル-2,4-シクロヘキサンジイソシアネート、メチル-2,6-シクロヘキサンジイソシアネート、4,4’-メチレンビス(シクロヘキシルイソシアネート)、1,4-ビス(イソシアネートメチル)シクロヘキサン、1,4-ビス(イソシアネートメチル)シクロヘキサン等が挙げられる。
なお、これらの多価イソシアネート化合物(x2)は、上記ポリイソシアネートのトリメチロールプロパンアダクト型変性体、水と反応させたビュウレット型変性体、イソシアヌレート環を含有させたイソシアヌレート型変性体であってもよい。
脂肪族ジオールとしては、例えば、1,3-プロパンジオール、1,4-ブタンジオール、1,5-ペンタンジオール、ネオペンチルグリコール、1,6-ヘキサンジオール、1,7-ヘプタンジオール等のアルカンジオール、エチレングリコール、プロピレングリコール、ジエチレングリコール、ジプロピレングリコール等のアルキレングリコールが挙げられる。
脂肪族ジアミンとしては、例えば、エチレンジアミン、1,3-プロパンジアミン、1,4-ブタンジアミン、1,5-ペンタンジアミン、1,6-ヘキサンジアミン等が挙げられる。
アルカノールアミンとしては、例えば、モノエタノールアミン、モノプロパノールアミン、イソプロパノールアミン等が挙げられる。
ビスフェノールとしては、例えば、ビスフェノールA等が挙げられる。
芳香族ジアミンとしては、例えば、ジフェニルメタンジアミン、トリレンジアミン、キシリレンジアミン等が挙げられる。
使用する触媒としては、特に制限はないが、3級アミン系化合物、有機金属系化合物等が挙げられる。
(x1)成分と(x2)成分の配合比については、NCO基とOH基とのモル比(〔NCO基〕/〔OH基〕)が、好ましくは1.1~3.0、より好ましくは1.2~2.5となるように反応させることが好ましい。
また、得られるウレタン系プレポリマー(α1)中のイソシアネート基含有量(NCO%)は、JIS K 1603-1に準じて測定された値において、好ましくは0.5~12質量%、より好ましくは1~4質量%である。
・ウレタン系プレポリマー(α1)の溶液を反応器に仕込み、その反応器に鎖延長剤(x3)を滴下して反応させる方法。
・鎖延長剤(x3)を反応器に仕込み、そこにウレタン系プレポリマー(α1)の溶液を滴下して反応させる方法。
・ウレタン系プレポリマー(α1)を溶剤で希釈した溶液を反応器に仕込み、そこに鎖延長剤を所定量一括投入して反応させる方法。
イソシアネート基と反応可能な活性水素を1つだけ有する化合物としては、例えば、メタノール、エタノール等のモノオール化合物等が挙げられる。
アミノ基を1つだけ有する化合物としては、例えば、ジエチルアミン、モルホリン等が挙げられる。
本発明で使用する樹脂部分(A)を形成する樹脂組成物において、封止シートの粘着力を向上させる観点から、樹脂部分(A)を形成する樹脂組成物は、さらに粘着付与剤を含むことができる。
具体的な粘着付与剤としては、後述する樹脂部分(B)を形成する樹脂組成物で記載する粘着付与剤が挙げられる。
樹脂部分(A)を形成する樹脂組成物と共に使用することができる粘着付与剤の軟化点は、好ましくは60~170℃、より好ましくは65~160℃、更に好ましくは70~150℃である。なお、「軟化点」は、JIS K 2207に準拠して測定した値である。
樹脂部分(A)を形成する樹脂組成物中に、上述の官能基含有モノマー(p2)由来の構成単位(p2)を有するアクリル系樹脂等の上述の官能基を有する樹脂を含有する場合、樹脂部分(A)を形成する樹脂組成物は、さらに架橋剤を含有することが好ましい。架橋剤は、上記樹脂の官能基と反応して、樹脂同士を架橋するものである。
架橋剤としては、例えば、トリレンジイソシアネート、ヘキサメチレンジイソシアネート等、及びそれらのアダクト体等のイソシアネート系架橋剤;エチレングリコールグリシジルエーテル等のエポキシ系架橋剤;ヘキサ〔1-(2-メチル)-アジリジニル〕トリフオスファトリアジン等のアジリジン系架橋剤;アルミニウムキレート等のキレート系架橋剤;等が挙げられる。これらの架橋剤は、単独で又は2種以上を組み合わせて用いてもよい。
これらの中でも、凝集力を高めて界面密着力を向上させる観点、及び入手し易さ等の観点から、イソシアネート系架橋剤が好ましい。
樹脂部分(A)を形成する樹脂組成物には、本発明の効果を損なわない範囲において、封止シートの用途に応じて、その他の添加剤を含有させてもよい。その他の添加剤としては、例えば、紫外線吸収剤、酸化防止剤、軟化剤(可塑剤)、充填剤、防錆剤、顔料、染料等が挙げられる。
これらの添加剤を配合する場合、添加剤の配合量は、樹脂部分(A)を形成する樹脂組成物100質量部に対して、好ましくは0.01~6質量部である。
本発明で使用する樹脂部分(B)の、JIS K 7129に準拠して測定した水蒸気透過率は15g/m2/day以下である。
水蒸気透過率が15g/m2/dayを超えると、加温・加湿条件下や、長期の使用において、樹脂部分(B)を有する封止シート中への水分の浸入を効果的に防ぐことができない。同様の観点から、樹脂部分(B)を形成する樹脂組成物の水蒸気透過率は、好ましくは14g/m2/day以下、より好ましくは13g/m2/day以下、更に好ましくは10g/m2/day以下、より更に好ましくは5g/m2/day以下、より更に好ましくは4g/m2/day以下である。
なお、当該水蒸気透過率の値は、実施例に記載の方法により測定した値を意味する。
この中でも、ポリイソブチレン系樹脂を含むことがより好ましい。
ポリイソブチレン系樹脂の構造は、主鎖又は側鎖にポリイソブチレン骨格を有する樹脂であり、下記の構成単位(b)を有する樹脂である。
なお、ポリイソブチレン系樹脂が共重合体である場合、イソブチレンからなる構成単位が、全モノマー成分の中で一番多く含まれているものとする。
これらの中でも、高耐久性及び高耐候性、並びに水蒸気透過率を低下させる観点から、重合した際に密な分子構造を有し、主鎖及び側鎖に重合性二重結合を残さないイソブチレンからなる構成単位を含むものが好ましい。
イソブチレンからなる構成単位の含有量は、樹脂に含まれる全構成単位に対して、好ましくは80~100質量%、より好ましくは90~100質量%、更に好ましくは100質量%である。
市販品としては、Vistanex(Exxon Chemical Co.製)、Hycar(Goodrich社製)、Oppanol(BASF社製)等が挙げられる。
前記ポリイソブチレン系樹脂(b-1)は、質量平均分子量が27万~60万であるポリイソブチレン系樹脂である。特定の質量平均分子量を有するポリイソブチレン系樹脂(b-1)を含有することで、封止シートの耐久性及び耐候性を向上させると共に、水蒸気透過率を低下させることができる。
樹脂(b-1)の質量平均分子量が27万以上であれば、得られる樹脂組成物の凝集力を十分向上させることができ、当該樹脂組成物を用いた封止シートの粘着力、及び水分浸入の抑制効果を向上させることができる。また、被着体への汚染の懸念も解消し得る。基本的に、質量平均分子量が高いほど、水蒸気透過率を低下させ、保持力を向上させることができる。
一方、樹脂(b-1)の質量平均分子量が60万以下であれば、得られる樹脂組成物の凝集力が高くなりすぎることにより柔軟性や流動性の低下という弊害を避けることができ、当該樹脂組成物から形成される樹脂層の被着体との濡れを良好にすることができる。また、樹脂組成物を溶液の形態とする際、溶媒に対する溶解性を良好とすることができる。
前記ポリイソブチレン系樹脂(b-2)は、質量平均分子量が5万~25万のポリイソブチレン系樹脂である。特定の質量平均分子量を有するポリイソブチレン系樹脂(b-2)を含有することで、被着体の種類によらず優れた粘着力を付与できると共に、粘着力と保持力のバランスが向上する。
ポリイソブチレン系樹脂(b-2)の構造は、樹脂(b-1)と同様に、主鎖又は側鎖にポリイソブチレン骨格を有する樹脂であり、上記の構成単位(b)を有する樹脂である。
樹脂(b-2)としては、上述の樹脂(b-1)で例示したものが挙げられるが、高耐久性及び高耐候性、並びに水蒸気透過率を低下させる観点から、重合した際に密な分子構造を有し、主鎖及び側鎖に重合性二重結合を残さないイソブチレンからなる構成単位を含むものが好ましい。
イソブチレンからなる構成単位の含有量は、樹脂(b-2)に含まれる全構成単位に対して、好ましくは80~100質量%、より好ましくは90~100質量%、更に好ましくは100質量%である。
なお、樹脂(b-2)は、単独で又は2種以上を組み合わせて用いてもよい。また、樹脂(b-2)の合成方法、及び使用できる市販品についても、上述の樹脂(b-1)と同様である。
樹脂(b-2)の質量平均分子量は、樹脂(b-1)と良好に相溶し適度に樹脂(b-1)を可塑化させると共に、水蒸気透過率等の他の物性への影響を抑える観点から、5万~25万であるが、好ましくは10万~25万、より好ましくは12万~23万、更に好ましくは15万~22万、より更に好ましくは18万~21万である。
樹脂(b-2)の質量平均分子量が5万以上であれば、得られる樹脂組成物から形成される樹脂層において、樹脂(b-2)が低分子成分として分離して樹脂層の表面に析出し、被着体が汚染される弊害を防ぐことができる。また、高温下で発生するアウトガス発生量が増加する等の物性に及ぼす影響も回避することができる。
一方、樹脂(b-2)の質量平均分子量が25万以下であれば、樹脂(b-2)を十分に可塑化させることができ、得られる樹脂組成物から形成される樹脂層の被着体との濡れを良好にすることができる。
当該含有量が5質量部以上であれば、樹脂(b-1)を十分に可塑化させることができ、被着体との濡れが十分に得られ、粘着力が優れる。一方、当該含有量が55質量部以下であると、凝集力が低下せずに粘着力及び保持力を維持できると共に、紫外線照射に対する耐久性にも優れる。
前記ポリイソブチレン系樹脂(b-3)は、質量平均分子量が2万以上のポリイソブチレン系樹脂である。
樹脂(b-3)の質量平均分子量が2万以上であると、樹脂組成物の凝集力が十分に得られ、粘着性を十分に向上させることができる。また、樹脂組成物を用いた封止シートを用いた際、封止シートの水分浸入の抑制効果も十分である。さらに、被着体を汚染してしまうことを防止できる。
なお、基本的には、樹脂(b-3)の質量平均分子量が高いほど、得られる樹脂組成物を用いた封止シートの粘着力を向上させ、当該封止シートを封止用途に用いた際の水分浸入の抑制効果も向上する傾向にある。
樹脂(b-3)の質量平均分子量は、2万以上であるが、上記観点、及び被着体に対する濡れ性や溶媒に対する溶解性の観点から、好ましくは3万~100万、より好ましくは5万~80万、更に好ましくは7万~60万、より更に好ましくは14万~45万である。
本発明で使用する樹脂部分(B)を形成する樹脂組成物は、スチレン-ブタジエン-スチレントリブロック共重合体(SBS)、スチレン-(エチレン-co-ブチレン)-スチレントリブロック共重合体(SEBS)、スチレン-イソブチレンジブロック共重合体(SIB)、及びスチレン-イソブチレン-スチレントリブロック共重合体(SIBS)から選ばれる1種以上のスチレン系共重合体(b-4)を含むことが好ましい。
樹脂部分(B)を形成する樹脂組成物中に、樹脂(b-4)として、上記より選ばれる1種以上のスチレン系共重合体を含有することで、当該樹脂組成物を用いた封止シートの水分浸入の抑制効果を良好とすると共に、当該封止シートの粘着力を向上させることができる。
樹脂(b-4)の中でも、当該樹脂組成物を用いた封止シートの粘着力を向上させる観点から、SBS及びSEBSから選ばれる1種以上が好ましい。また、当該封止シートの水分浸入の抑制効果を向上させる観点から、SIB及びSIBSから選ばれる1種以上が好ましい。
(b-4)成分のMwが1万以上であれば、得られる樹脂組成物を用いた封止シートの粘着力を向上させることができる。一方、(b-4)成分のMwが40万以下であれば、得られる樹脂組成物を用いた封止シートの粘着力を良好に保ちつつ、得られる樹脂組成物から形成される樹脂層の水蒸気透過率の値を小さくすることができ、封止シートの水分浸入の抑制効果を向上させることができる。
当該含有量比が上記の範囲内であれば、得られる樹脂組成物を用いた封止シートの粘着力を向上させつつ、及び当該樹脂組成物から形成される樹脂層の水蒸気透過率の値を小さくし、封止シートの水分浸入の抑制効果を良好とすることができる。
本発明で使用する樹脂部分(B)を形成する樹脂組成物が、更に、軟化点が135℃以下の粘着付与剤を含有することが好ましい。
粘着付与剤とは、樹脂部分(B)を形成する樹脂組成物やその他の樹脂成分と混合することが可能であり、これらの樹脂成分の粘着性能を向上させる機能を持つ、オリゴマー領域の分子量を有する化合物を意味する。粘着付与剤の数平均分子量としては、通常100~18000、好ましくは100~10000である。
粘着付与剤の軟化点が135℃以下であると、樹脂部分(B)を含む樹脂組成物の粘着性が著しく低下することを抑制できるため好ましい。また、当該樹脂組成物を用いた封止シートの剥離時に発生するジッピングを抑制することができる。
粘着付与剤の軟化点は、上記観点から、好ましくは132℃以下、より好ましくは128℃以下、更に好ましくは120℃以下、より更に好ましくは110℃以下、より更に好ましくは105℃以下である。
一方、得られる樹脂組成物の凝集力を向上させ、優れた粘着性を発現する樹脂組成物を得る観点から、粘着付与剤の軟化点は、好ましくは60℃以上、より好ましくは70℃以上、更に好ましくは80℃以上、より更に好ましくは90℃以上である。
本発明において、軟化点の異なる粘着付与剤を2種以上組み合わせてもよい。複数の粘着付与剤を用いる場合、これらの粘着付与剤の軟化点の加重平均が上記範囲に属していればよい。そのため、本発明において、複数の粘着付与剤の軟化点の加重平均が135℃以下であれば(上記範囲に属していれば)、軟化点が135℃を超える粘着付与剤を樹脂部分(B)を形成する樹脂組成物中に含有してもよい。
軟化点が135℃を超える粘着付与剤の含有量は、樹脂部分(B)を形成する樹脂組成物中に含まれる粘着付与剤の全量に対して、好ましくは10質量%以下、より好ましくは4質量%以下、更に好ましくは1質量%以下、より更に好ましくは0.01質量%以下である。
上記粘着付与剤は、単独または2種以上を組み合わせて用いてもよい。
ここで、上記の「C5留分」とは、石油ナフサの熱分解で生成する、ペンテン、イソプレン、ピペリン、1.3-ペンタジエン等の炭素数5の不飽和炭化水素を意味し、「C5系石油樹脂」とは、このC5留分を共重合して得られ、C5留分を主成分(少なくとも20質量%以上含む)とする樹脂を意味する。
また、上記の「C9留分」とは、石油ナフサの熱分解で生成する、インデン、ビニルトルエン、α又はβ-メチルスチレン等の炭素数9の不飽和炭化水素を意味し、「C9系石油樹脂」とは、このC9留分を共重合して得られ、C9留分を主成分(少なくとも20質量%以上含む)とする樹脂を意味する。
なお、上記の「水素化した樹脂」は、完全に水素化した完全水素化樹脂だけでなく、一部が水素化された部分水素化樹脂も含まれる。
当該粘着付与剤の含有量が5質量部以上であれば、得られる樹脂組成物から形成される樹脂層について、被着体との濡れが十分に得られ、粘着力を向上させることができると共に、当該樹脂層の水蒸気透過率の値が小さく、水分浸入の抑制効果に優れた封止シートを得ることができる。
一方、当該粘着付与剤の含有量が60質量部以下であれば、得られる樹脂組成物から形成される樹脂層について、被着体によらず優れた粘着力を発現させることができ、ジッピングの発生を抑制することができる。また、当該樹脂層の水蒸気透過率の値が小さく、水分浸入の抑制効果に優れた封止シートを得ることができる。
本発明の樹脂部分(B)を形成する樹脂組成物は、本発明の効果を阻害しない範囲において、更にその他の添加剤を含有してもよい。
その他の添加剤としては、例えば、前述の樹脂部分(A)を形成する樹脂組成物中で記載したその他の添加剤が挙げられる。その他の添加剤は、単独で又は2種以上を組み合わせて用いてもよい。
支持体としては、シート形状であれば特に限定されず、本発明の封止シートの使用目的に応じて適宜選定される。例えば、上質紙、アート紙、コート紙、グラシン紙等や、これらの紙基材にポリエチレン等の熱可塑性樹脂をラミネートしたラミネート紙等の各種紙類、各種合成紙、アルミニウム箔や銅箔や鉄箔等の金属箔、不織布等の多孔質材料、並びにポリエチレン樹脂、ポリプロピレン樹脂等のポリオレフィン樹脂、ポリブチレンテレフタレート樹脂、ポリエチレンテレフタレート樹脂等のポリエステル樹脂、アセテート樹脂、ABS樹脂、ポリスチレン樹脂、塩化ビニル樹脂等のプラスチックのフィルム、シート及びこれらの樹脂の混合物又は積層物からなるプラスチックフィルム、シート等が挙げられる。プラスチックフィルム・シート等のシート形状の基材は、未延伸でもよいし、縦又は横等の一軸方向あるいは二軸方向に延伸されていてもよい。
使用する支持体は、着色の有無については問わないが、封止用部材として用いるため、紫外線を十分に透過するものが好ましく、さらに可視光領域においても無色透明であることがより好ましい。
また、本発明の封止シートにおいて、上述の材料からなる支持体の代わりに、ガスバリア用基材とガスバリア層を有するガスバリアフィルムを支持体として用いてもよい。ガスバリアフィルムの詳細は、後述のとおりである。
酸化法としては、特に限定されず、例えば、コロナ放電処理法、プラズマ処理法、クロム酸酸化(湿式)、火炎処理、熱風処理、オゾン・紫外線照射処理等が挙げられる。また、凹凸化法としては、特には限定されず、例えば、サンドブラスト法、溶剤処理法等が挙げられる。
これらの表面処理は、支持体の種類に応じて適宜選定されるが、樹脂層との接着性の向上効果や操作性の観点から、コロナ放電処理法が好ましい。また、プライマー処理を施すこともできる。
このような目止め層としては、特に限定されないが、例えは、スチレン-ブタジエン共重合体、アクリル系樹脂、ポリエステル系樹脂、ポリウレタン系樹脂、ポリスチレン系樹脂等を主成分(少なくとも20質量%以上含有する)として、必要に応じ、クレー、シリカ、炭酸カルシウム、酸化チタン、酸化亜鉛等のフィラーを添加したもの等からなる層が挙げられる。
この目止め層の厚さは、特に制限はないが、通常0.1~30μmである。
本発明の封止シートの支持体としては、ガスバリア用基材とガスバリア層とを有するガスバリアフィルムを用いることが好ましい。当該ガスバリアフィルムは、ガスバリアフィルム用基材の少なくとも一方の面側にガスバリア層を有するものであればよい。
また、ガスバリアフィルムは、無機層、有機層及び金属層から選ばれる1種以上からなる単層又は複数層のガスバリア層を有することが好ましい。
ガスバリアフィルム用基材としては、特に制限されず、例えば、ポリエチレン、ポリプロピレン等のポリオレフィン、ポリエチレンテレフタレート、ポリブチレンテレフタレート等のポリエステル、ポリイミド、ポリアミドイミド、全芳香族ポリアミド、ナイロン6、ナイロン66、ナイロン共重合体等のポリアミド、ルボルネン系重合体、単環の環状オレフィン系重合体、環状共役ジエン系重合体、ビニル脂環式炭化水素重合体、及びこれらの水素化物等のシクロオレフィン系ポリマー等、ポリフェニレンエーテル、ポリエーテルケトン、ポリエーテルエーテルケトン、ポリカーボネート、ポリスルフォン、ポリエーテルスルフォン、ポリフェニレンスルフィド、ポリアリレートの樹脂からなるシート等が挙げられる。
これらの中でも、透明性に優れ、汎用性の観点から、ポリエステル、ポリアミド又はシクロオレフィン系ポリマーが好ましく、ポリエステル又はシクロオレフィン系ポリマーがより好ましい。
ガスバリア層を形成する材料としては、酸素及び水蒸気の透過を阻止するものであれば、特に制約されないが、ガスバリア層に無機層を有する場合には、無機層は、ダイヤモンドライクガラス、ダイヤモンドライクカーボン、ケイ素酸化物、ケイ素窒化物及びケイ素炭化物から選ばれる1種以上を含む無機材料から形成されたものであることが好ましい。ガスバリア層に有機層を有する場合には、有機層は、ポリイミド、ポリアミド、ポリアミドイミド、ポリフェニレンエーテル、ポリエーテルケトン及びポリエーテルエーテルケトンから選ばれる1種以上を含む有機材料から形成されたものであることが好ましい。
ガスバリア層の厚みは、好ましくは10~2000nmであり、より好ましくは50~500nmである。
ガスバリアフィルム用基材の上にガスバリア層を形成する場合には、該基材の上に、アンカー層を設けることが好ましく、アンカー層の厚みは、好ましくは1~2000nmであり、より好ましくは1~1000nmである。アンカー層を構成する材料としては、例えばアクリル樹脂やポリエステル樹脂等が挙げられる。
剥離シートとしては、両面剥離処理をされた剥離シートや、片面剥離処理された剥離シート等が用いられ、剥離シート用基材上に剥離剤を塗布したもの等が挙げられる。
剥離シート用の基材としては、例えば、グラシン紙、コート紙、上質紙等の紙基材、これらの紙基材にポリエチレン等の熱可塑性樹脂をラミネートしたラミネート紙、又はポリエチレンテレフタレート樹脂、ポリブチレンテレフタレート樹脂、ポリエチレンナフタレート樹脂等のポリエステル樹脂フィルム、ポリプロピレン樹脂、ポリエチレン樹脂等のポリオレフィン樹脂フィルム等のプラスチックフィルム等が挙げられる。
剥離剤としては、例えば、シリコーン系樹脂、オレフィン系樹脂、イソプレン系樹脂、ブタジエン系樹脂等のゴム系エラストマー、長鎖アルキル系樹脂、アルキド系樹脂、フッ素系樹脂等が挙げられる。
剥離シートの厚さは、特に制限ないが、好ましくは20~200μm、より好ましくは25~150μmである。
本発明の封止シートの製造方法としては、特に制限はなく、公知の方法により製造することができる。例えば、上述の樹脂組成物に有機溶媒を加えた樹脂組成物の溶液を公知の塗布方法により製造する方法が挙げられる。
有機溶媒を配合した場合の樹脂部分(A)を形成する樹脂組成物の溶液の固形分濃度、及び樹脂部分(B)を形成する樹脂組成物の溶液の固形分濃度は、各々、好ましくは10~60質量%、より好ましくは10~45質量%、更に好ましくは15~30質量%である。当該固形分濃度が10質量%以上であれば、有機溶媒の使用量としては十分であり、60質量%以下であれば、適度な粘度となり、優れた塗布作業性を有する溶液となり得る。
本発明の封止シートは、優れた界面密着力及び被着体との界面密着性を有し、特に水分浸入の抑制効果に優れている。
そのため、本発明の封止シートは、有機EL素子等の封止用部材として好適であり、本発明の封止シートを封止用部材として用いた場合、水分浸入や有機EL素子の駆動時の発熱による封止シートの基板(被着体)と封止シートとの密着性低下を抑制することができ、有機EL素子の特性劣化を抑えることができる。
これらの中でも、本発明の封止シートは、有機EL素子の封止用途として用いられることが好ましい。
本発明の封止構造体は、基板(被着体)上に設けられた被封止体を本発明の封止シートにより封止してなる封止構造体である。
本発明の封止シートにより封止した封止構造体の実施態様に係る封止構造体の例を、図3及び図4を用いて説明するが、本発明の封止構造体は、本発明の効果が発現する限り、以下の例に限定されるものではない。なお、図3及び図4中の平面図は、説明のために支持体5及び基板(被着体)9の記載を省略した封止構造体の一部分を示す平面図である。
図3(b)の断面図に示す一態様は、図3(a)上のX-X’上における断面図が取り得る一例を示している。図3(b)の断面図において、封止構造体301(b)は、基板(被着体)9上に樹脂層4及び支持体5からなる封止シート8が設けられた構造であり、基板(被着体)9上に被封止物7が配置され、被封止物7を封止する樹脂部分(B)2の両端に樹脂部分(A)1が存在している。該樹脂部分(A)1は、基板(被着体)9及び支持体5のいずれにも接している。
また、図3(c)の断面図に示す一態様は、図3(a)上のX-X’上における断面図が取り得る一例を示している。図3(c)の断面図において、封止構造体301(c)は、基板(被着体)9上に樹脂層4及び支持体5からなる封止シート8が設けられた構造であり、基板(被着体)9上に被封止物7が配置され、被封止物7を封止する樹脂部分(B)2の両端に樹脂部分(A)1が存在している。該樹脂部分(A)1は、基板(被着体)9にのみ接している。支持体5側には、被封止物7を封止する樹脂部分(B)2のみが接している。
図4(b)の断面図に示す一態様は、図4(a)上のX-X’上における断面図が取り得る一例を示している。図4(a)の断面図において、封止構造体302(b)は、基板(被着体)9上に樹脂層4及び支持体5からなる封止シート8が設けられた構造であり、基板(被着体)9上に被封止物7が配置され、樹脂部分(B)2により被封止物7が封止されており、基板(被着体)9が被封止物7と接している表面上において、被封止物7の外縁部から基板(被着体)9の外縁部に向かう直線上に樹脂部分(B)2と樹脂部分(A)1と樹脂部分(B)2とがこの順で存在している。そして、該樹脂部分(A)1が、基板(被着体)9及び支持体5のいずれにも接している。
また、図4(c)の断面図に示す一態様は、図4(a)上のX-X’上における断面図が取り得る一例を示している。図4(c)の断面図において、封止構造体302(c)は、基板(被着体)9上に樹脂層4及び支持体5からなる封止シート8が設けられた構造であり、基板(被着体)9上に被封止物7が配置され、樹脂部分(B)2により被封止物7が封止されており、基板(被着体)9が被封止物7と接している表面上において、被封止物7の外縁部から基板(被着体)9の外縁部に向かう直線上に樹脂部分(B)2と樹脂部分(A)1と樹脂部分(B)2とがこの順で存在している。そして、該樹脂部分(A)1は、基板(被着体)9にのみ接している。支持体5側には、被封止物7を封止する樹脂部分(B)2のみが接している。
本発明の封止構造体が有する基板(被着体)は、例えば、ガラス板やガスバリアフィルムが使用される。ガラス板は、従来電子デバイス用に用いられているものが使用できる。ガスバリアフィルムは、前記封止シートで上述したガスバリアフィルムと同一のフィルムを用いることができる。
基板(被着体)の厚みは、好ましくは1~300μmであり、より好ましくは20~200μmである。
基板(被着体)は、JIS K 7129に準拠して測定される、40℃、90%RH(相対湿度)条件下での水蒸気透過率が、0.1g/m2/day未満であることが好ましく、0.01g/m2/day未満であることがより好ましい。
なお、基板(被着体)の水蒸気透過率は、後述する実施例に記載のガス透過率測定装置を使用して測定することができる。
本発明の封止構造体が封止する被封止物は、前記封止シートで上述したのと同様に、有機EL素子等であることが好ましい。本発明の封止構造体では、水分浸入や有機EL素子の駆動時の発熱による封止シートと基板(被着体)との密着性低下を抑制することができ、有機EL素子の特性劣化を抑えることができる。
同様に、被封止物が有機ELディスプレイ素子、液晶ディスプレイ素子、太陽電池素子であると、本発明の封止構造体の効果が、より発揮されるために好ましい。
本発明の封止シート又は封止構造体を有する、発光装置、表示装置又は太陽電池は、水分浸入や各素子の駆動時の発熱による封止シートと基板(被着体)との密着性低下を抑制することができ、各素子の特性劣化を抑えることができるため、加温・加湿条件下での耐久性に優れる。
特に、本発明の封止シート又は封止構造体を有する有機EL、有機ELディスプレイでは、水分浸入や有機EL素子の駆動時の発熱による封止シートと基板(被着体)との密着性低下を抑制することができ、有機EL素子の特性劣化を抑えることができ、加温・加湿条件下での耐久性に優れる。同様に、本発明の封止シート又は封止構造体を有する、液晶ディスプレイ、太陽電池も加温・加湿条件下での耐久性に優れる。
ゲル浸透クロマトグラフ装置(東ソー株式会社製、製品名「HLC-8020」)を用いて、下記の条件下で測定し、標準ポリスチレン換算にて測定した値を用いた。
(測定条件)
・カラム:「TSK guard column HXL-H」「TSK gel GMHXL(×2)」「TSK gel G2000HXL」(いずれも東ソー株式会社製)
・カラム温度:40℃
・展開溶媒:テトラヒドロフラン
・流速:1.0mL/min
JIS K 2207に準拠して測定した値を用いた。
(製造例1)アクリル系樹脂組成物Aの製造
樹脂部分(A)を形成する樹脂組成物は、以下の方法にて調製した。
単量体成分として、アクリル酸ブチル90質量部及びアクリル酸10質量部、重合開始剤として、アゾビスイソブチロニトリル0.2質量部を反応器に入れ混合した。そして、4時間窒素ガスで脱気を行い、60℃まで徐々に昇温した後、24時間撹拌しながら重合反応を行ない、アクリル系共重合体(Mw=65万)含有酢酸エチル溶液(固形分濃度33質量%)を得た。
得られたアクリル系共重合体含有酢酸エチル溶液100質量部(固形分)に、イソシアネート系架橋剤(日本ポリウレタン株式会社製、製品名「コロネートL」、トリメチロールプロパン変性トリレンジイソシアネートの酢酸エチル溶液、固形分75質量%)1.5質量部(固形分比)を添加してトルエンに溶解し、固形分濃度20質量%のアクリル系樹脂組成物Aの溶液を調製した。
樹脂部分(B)を形成する樹脂組成物は、以下の原料を使用した。
・「Oppanol B100」(商品名、BASF社製):ポリイソブチレン系樹脂、Mw=100万
・「Oppanol B50」(商品名、BASF社製):ポリイソブチレン系樹脂、Mw=34万
・「Oppanol B30」(商品名、BASF社製):ポリイソブチレン系樹脂、Mw=20万
・「Kraton G1726」(商品名、クレイトンポリマー社製):SEBS(Mw=7万)/SEB(Mw=3.5万)=30/70(質量比)の割合で含有するスチレン系共重合体混合物、スチレン含有量30質量%
・「アイマーブ P-100」(商品名、出光興産株式会社製):ジシクロペンタジエンと芳香族ビニルモノマーとの共重合体の水添石油樹脂、軟化点100℃
・「アルコン P-125」(商品名、荒川化学工業株式会社製):脂環族飽和炭化水素樹脂、軟化点115℃
・「Quinton R-100」(商品名、日本ゼオン株式会社製):脂肪族系炭化水素樹脂、軟化点96℃
表1に示す実施例及び比較例において調製した樹脂組成物(B)のトルエン溶液を、スクリーン印刷機にて重剥離フィルムとして表面がシリコーン剥離処理されたポリエチレンテレフタレートフィルム(リンテック株式会社製、製品名「SP-PET38T103-1」、厚み38μm)上に、乾燥後の厚さが50μmになるように塗布し、120℃で2分間乾燥させて樹脂部分(B)のみからなる樹脂層を形成させて、形成した樹脂層面に、軽剥離フィルムとして、表面がシリコーン剥離処理されたポリエチレンテレフタレートフィルム(リンテック株式会社製、製品名「SP-PET381130」、厚み38μm)の剥離処理面を貼付し、2枚の剥離フィルムに挟持された基材無しの樹脂部分(B)のみからなる樹脂層を有するシートを得た。
このシートの2枚の剥離フィルムを剥離して表出した樹脂層の面上に、ポリエチレンテレフタレートフィルム(三菱樹脂株式会社製、厚さ6μm)でラミネートし、2枚のポリエチレンテレフタレートフィルムで挟まれた樹脂層からなる水蒸気透過率測定用のサンプルとした。
水蒸気透過率の測定は、JIS K 7129に準拠し、透過率測定器(LYSSY社製、製品名「L89-500」)を用いて、40℃、90%RH(相対湿度)の環境下で測定した。なお、ラミネートに用いたポリエチレンテレフタレートフィルムの水蒸気透過率は2枚で43g/m2/dayであった。つまり、樹脂層の水蒸気バリア性が全くゼロであれば、43g/m2/day前後の値を示す。当該値が低いほど、樹脂層の水蒸気バリア性が優れている。
表1記載の処方に従って、前記製造例1で得た樹脂部分(A)に用いる樹脂組成物のトルエン溶液と、樹脂部分(B)に用いる樹脂組成物のトルエン溶液を作成した。それぞれの溶液をスクリーン印刷機にて重剥離フィルム(リンテック株式会社製、製品名「SP-PET38T103-1」を、240mm×240mmにカット)の剥離処理面に乾燥後の厚さが50μmとなるように格子状(図1(a))に示す形状において、樹脂部分(A)の線幅が20mmとなるように塗布し、100℃で2分間乾燥して樹脂層の樹脂部分(A)を形成した。次いで、同様に中央部の樹脂部分(B)の一辺が100mmとなるように塗布して100℃で2分間乾燥して樹脂層の樹脂部分(B)を形成した。その際、当該樹脂層の両面に樹脂部分(A)及び樹脂部分(B)が同様に存在するように塗布した。さらに得られた樹脂層面上に、軽剥離フィルム(リンテック株式会社製、製品名「SP-PET381031」)を積層して、2枚の剥離フィルムで挟持し、23℃、50%RHで7日間シーズニングを行うことにより樹脂層が保護された封止シートを作成した。
そして、作成した封止シートの軽剥離シートを剥離除去して、表出した樹脂層にガスバリアフィルムをラミネートして、ガスバリアフィルムが積層した封止シートを作成した。
なお、ここで用いたガスバリアフィルムは、以下の方法にて作製した。支持基材は、厚さ100μmのポリエステルフィルムの一方の面上に、厚さ100nmのアクリル樹脂からなるアンカー層を設け、次いで、当該アンカー層上に厚さ100nmのケイ素酸化物からなる無機層を設けたガスバリアフィルムを用いた。
次に、基板(被着体)としてのガラス板上(算術平均粗さRa:2nm、最大突起高さRp:18nm)に、陽極、正孔輸送層、発光層、及び陰極を順次形成して、陽極/正孔輸送層/発光層/陰極の構造からなる有機ELディスプレイ素子(被封止物)を設けた。この陽極は、ITOをスパッタリング法で成膜した後、エッチングによりパターンニングして形成した。また、正孔輸送層は、α-ナフチルフェニルジアミンを用いて蒸着法により形成した。上記発光層は、トリス(8-キノリノール)アルミニウムを用いて形成した。上記陰極は、カルシウム及び銀を用いて蒸着法により二層構造の陰極を形成した。
そして、作成したガスバリアフィルムが積層した封止シートの重剥離シートを剥離除去して露出した樹脂層を、作製した基板(被着体)上の被封止物が密封されるように常温で貼り付けることにより封止構造体を作製した。
実施例1において、格子状に塗布する代わりに、図1(b)に示す形状において、樹脂部分(B)の線幅が20mmとなるように塗布した以外は、実施例1と同様の方法にて封止構造体を作製した。なお、当該樹脂層の両面に樹脂部分(A)及び樹脂部分(B)が同様に存在するように塗布した。
実施例1において、格子状に塗布する代わりに、図1(c)に示す形状において、樹脂部分(A)の線幅が20mmとなるように塗布した以外は、実施例1と同様の方法にて封止構造体を作製した。なお、当該樹脂層の両面に樹脂部分(A)及び樹脂部分(B)が同様に存在するように塗布した。
表1に記載の樹脂部分(B)に用いる樹脂組成物の処方を用いた以外は、実施例1と同様の方法にて封止構造体を作製した。
表1に記載の樹脂部分(B)に用いる樹脂組成物の処方を用いて、以外は、実施例1と同様の方法にて封止構造体を作製した。
前記製造例1で得た樹脂部分(A)に用いる樹脂組成物は用いず、表1に記載の樹脂部分(B)に用いる樹脂組成物のみを塗布して樹脂層を形成した以外は、実施例1と同様の方法にて封止構造体を作製した。
前記製造例1で得た樹脂部分(B)に用いる樹脂組成物は用いず、表1に記載の樹脂部分(A)に用いる樹脂組成物のみを塗布して樹脂層を形成した以外は、比較例1と同様の方法にて封止構造体を作製した。
表1に記載の実施例及び比較例で作製した封止構造体を、40℃、90%RH(相対湿度)に設定した恒温恒湿器内にて、4週間、及び8週間、該条件下にて保管して取出した。取出した封止構造体について、駆動条件を10mA/cm2として、封止構造体を発光させて、発光部を実体顕微鏡を用いて、倍率25倍で観察し、ダークスポットの有無を観察した。封止能評価は、以下に示す基準により評価した。
・A:ダークスポットの数が0個。
・B:ダークスポットの数が1~3個。
・C:ダークスポットの数が4個以上。
そのため、本発明の封止シートは、例えば、有機EL素子、液晶ディスプレイ素子、又は太陽電池素子等を封止するのに好適に用いられる。さらに、例えば、前記素子を有する発光装置、表示装置又は太陽電池などの装置にも、該封止シート又は該封止構造体当該封止シートは好適に用いられる。
2 樹脂部分(B)
3 閉じた領域
4 樹脂層
5 支持体
6 剥離シート
7 被封止物
8 封止シート
9 基板(被着体)
101~106 封止シートの樹脂層表面
201~204 封止シートの断面
301(a) 封止構造体の平面
301(b)、301(c) 封止構造体の断面
302(a) 封止構造体の平面
302(b)、302(c) 封止構造体の断面
Claims (17)
- アクリル系樹脂及びウレタン系樹脂から選ばれる1種以上の樹脂を含む樹脂組成物より形成されてなる樹脂部分(A)と、JIS K 7129に準拠して測定した水蒸気透過率が15g/m2/day以下となる樹脂部分(B)とを含む樹脂層を有する封止シートであって、
前記樹脂層の少なくとも一方の表面上に、樹脂部分(A)と樹脂部分(B)とが存在している、封止シート。 - 前記樹脂層の少なくとも一方の表面上に、樹脂部分(A)又は樹脂部分(B)が閉じた領域を形成し、当該閉じた領域内に他方の樹脂部分が存在してなる、請求項1に記載の封止シート。
- 前記樹脂層の少なくとも一方の表面上で、樹脂部分(A)の合計表面積と樹脂部分(B)の合計表面積との比率〔(A)面積/(B)面積〕が10/90~90/10である、請求項1又は2に記載の封止シート。
- 支持体上に、前記樹脂層を有する、請求項1~3のいずれかに記載の封止シート。
- 前記樹脂層の支持体側の表面上には樹脂部分(B)のみが存在し、前記樹脂層の他方の表面上には樹脂部分(A)及び樹脂部分(B)が存在している、請求項4に記載の封止シート。
- 前記支持体が、ガスバリアフィルムである、請求項4又は5に記載の封止シート。
- 樹脂部分(B)を形成する樹脂組成物が、ブチルゴム、ポリイソブチレン系樹脂、スチレン系共重合体、ポリイソプレン系樹脂、ポリブタジエン系樹脂及びポリブテン系樹脂から選ばれる1種以上の樹脂を含む、請求項1~6のいずれかに記載の封止シート。
- 樹脂部分(B)を形成する樹脂組成物が、質量平均分子量27万~60万のポリイソブチレン系樹脂(b-1)、及び質量平均分子量5万~25万のポリイソブチレン系樹脂(b-2)を含む、請求項7に記載の封止シート。
- 樹脂部分(B)を形成する樹脂組成物が、質量平均分子量が2万以上のポリイソブチレン系樹脂(b-3)、並びにスチレン-ブタジエン-スチレントリブロック共重合体(SBS)、スチレン-(エチレン-co-ブチレン)-スチレントリブロック共重合体(SEBS)、スチレン-イソブチレンジブロック共重合体(SIB)、及びスチレン-イソブチレン-スチレントリブロック共重合体(SIBS)から選ばれる1種以上のスチレン系共重合体(b-4)を含む、請求項7に記載の封止シート。
- スチレン系共重合体(b-4)の軟化点が、80~200℃である、請求項9に記載の封止シート。
- 樹脂部分(B)を形成する樹脂組成物が、更に、軟化点が135℃以下の粘着付与剤を含む、請求項1~10のいずれかに記載の封止シート。
- 有機EL素子の封止用として用いられる、請求項1~11のいずれかに記載の封止シート。
- 基板(被着体)上に設けられた被封止物を請求項1~12のいずれかに記載の封止シートにより封止してなる、封止構造体。
- 前記被封止物が、前記封止シートの表面上で樹脂部分(B)により閉じた領域内に位置する、請求項13に記載の封止構造体。
- 前記被封止物が、有機EL素子、有機ELディスプレイ素子、液晶ディスプレイ素子、又は太陽電池素子である、請求項13又は14に記載の封止構造体。
- 前記基板(被着体)が、ガラス板又はガスバリアフィルムである請求項13~15のいずれかに記載の封止構造体。
- 請求項1~12のいずれかに記載の封止シート、又は請求項13~16のいずれかに記載の封止構造体を有する、発光装置、表示装置又は太陽電池。
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CN201580011124.2A CN106062120A (zh) | 2014-03-27 | 2015-03-23 | 密封片、密封结构体及装置 |
US15/127,276 US20180170022A1 (en) | 2014-03-27 | 2015-03-23 | Sealing sheet, and sealing structure and device |
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JP2019077836A (ja) * | 2017-10-27 | 2019-05-23 | アイカ工業株式会社 | 封止用樹脂組成物 |
JP2019214152A (ja) * | 2018-06-12 | 2019-12-19 | 住友ベークライト株式会社 | 多層シート、トレイ及び包装体 |
WO2023181457A1 (ja) * | 2022-03-24 | 2023-09-28 | 株式会社Lixil | ロールスクリーン装置 |
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